CN110950564B - Phase change aggregate for self-sensing and self-cooling of asphalt pavement and preparation method thereof - Google Patents
Phase change aggregate for self-sensing and self-cooling of asphalt pavement and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1018—Coating or impregnating with organic materials
- C04B20/1029—Macromolecular compounds
- C04B20/1037—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
- C04B18/027—Lightweight materials
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Abstract
The invention discloses a phase change aggregate for self-perception and self-cooling of an asphalt pavement and a preparation method thereof, wherein the phase change aggregate comprises phase change ceramsite and an encapsulation layer coated on the phase change ceramsite; the packaging layer comprises the following components: the graphene oxide coating comprises polyethylene glycol, a cross-linking agent, isocyanate and graphene oxide, wherein the mass of the graphene oxide accounts for 1-5% of the total mass of the polyethylene glycol, the cross-linking agent and the isocyanate; of polyethylene glycol, crosslinking agent and isocyanate, [ NCO ]: the molar ratio of [ OH ] is 1.1 to 1.3, and in the crosslinking agent, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4-0.7. The polyurethane with the phase change function is prepared to encapsulate the phase change ceramsite, the raw materials and the synthesis formula of the polyurethane encapsulation layer of the phase change aggregate suitable for the asphalt pavement are selected, the graphene oxide containing rich hydroxyl groups is introduced into a polyurethane system through a chemical reaction, the dispersibility and the chemical stability of the graphene oxide in the polyurethane system are improved, the thermal conductivity of the phase change aggregate is fundamentally improved, and the preparation difficulty of the phase change aggregate is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of intelligent asphalt pavement materials, and particularly relates to a phase change aggregate for self-perception and self-cooling of an asphalt pavement and a preparation method thereof.
Background
In recent years, with the introduction of important strategies of "strong transportation" and the trend of people toward good life, the development of intelligent road infrastructure aiming at intelligent transportation in the future is more and more emphasized. The intelligent road infrastructure should have the intelligent service capabilities of road infrastructure such as active sensing, automatic resolution, autonomous regulation, etc.
The phase-change material is a material which changes the phase state within the phase-change temperature range, absorbs, stores or releases a large amount of heat in the form of latent heat, and the temperature of the material is kept unchanged. In recent years, researchers apply the asphalt pavement material to asphalt mixture to prepare the asphalt pavement material with the self-cooling function. The high-temperature action time of the asphalt pavement is shortened through the phase change heat storage characteristic in a high-temperature season, so that the temperature of the asphalt pavement is actively reduced, and the high-temperature diseases of the pavement are relieved; in addition, the phase-change asphalt pavement can also relieve the urban heat island effect.
Traditional phase change material becomes liquid in phase change energy storage process, needs to carry out the splendid attire with certain carrier to restriction liquid phase change material's flow makes composite phase change material keep macroscopic solid-state in the phase change in-process. Research shows that the porous matrix and the layered matrix are commonly used for containing the phase change substances, and the matrix into which the phase change substances are introduced is further encapsulated by adopting an epoxy curing process so as to prevent the phase change substances from seeping out of a carrier material when being melted to influence the service life and the adverse effect on the asphalt pavement. Nevertheless, the shaped phase change material after epoxy curing still has certain defects, which are mainly manifested by low overall latent heat, and is partly due to the low thermal conductivity of the epoxy encapsulation layer, which undoubtedly reduces the heat storage capacity and the temperature regulation capability of the shaped phase change material; meanwhile, because the thermal conductivity of the epoxy encapsulation layer is low, the thickness of the encapsulation layer needs to be strictly limited, so that the preparation difficulty of the shaped phase-change material is greatly improved; in addition, the prepared shaped phase change material is often added into asphalt mixture as phase change aggregate, however, in the construction process and service state of asphalt pavement, the aggregate needs to have enough strength to bear various load effects so as to meet the long-term performance of the pavement, which puts forward higher requirements on the strength of the phase change aggregate, so that how to balance the thickness of the epoxy encapsulation layer and the strength of the aggregate becomes a great problem when the phase change aggregate is prepared.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a phase change aggregate for self-perception and self-cooling of an asphalt pavement and a preparation method thereof, so as to overcome the defects in the prior art.
In order to solve the technical problems, the invention solves the problems by the following technical scheme:
a phase change aggregate for self-sensing and self-cooling of an asphalt pavement comprises phase change ceramsite and an encapsulation layer coated on the phase change ceramsite;
the packaging layer comprises the following components: the graphene oxide coating comprises polyethylene glycol, a cross-linking agent, isocyanate and graphene oxide, wherein the mass of the graphene oxide accounts for 1-5% of the total mass of the polyethylene glycol, the cross-linking agent and the isocyanate;
of polyethylene glycol, crosslinking agent and isocyanate, [ NCO ]: the molar ratio of [ OH ] is 1.1 to 1.3, and in the crosslinking agent, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4-0.7.
Further, the relative molecular weight of the polyethylene glycol is one or more of 4000-10000.
Further, the crosslinking agent is trifunctional glycerol.
Further, the isocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethyl diisocyanate.
A preparation method of a phase-change aggregate for self-perception and self-cooling of an asphalt pavement comprises the following steps:
step 1: heating the polyethylene glycol to a molten state;
step 2: adding the cross-linking agent and the graphene oxide into molten polyethylene glycol, and uniformly mixing to obtain a physical blending system containing hydroxyl to be reacted;
and step 3: adding the isocyanate and the diluent into the system obtained in the step 2, and reacting to obtain a polyurethane system;
and 4, step 4: adding the phase-change ceramsite into the polyurethane system obtained in the step (3), and taking out the phase-change ceramsite adhered with the polyurethane system to preliminarily cure the polyurethane system on the phase-change ceramsite;
and 5: and (4) drying the primarily solidified phase-change ceramsite obtained in the step (4) to obtain the phase-change aggregate.
Further, in the step 1, the heating temperature is 70-90 ℃, and the heating is carried out under the protection of inert gas; in the step 2, polyethylene glycol, a cross-linking agent and graphene oxide are uniformly mixed by stirring or ultrasonic dispersion.
Further, in the step 3, stirring for 5-10 min at 70-90 ℃, and then cooling to 45-50 ℃; the diluent is a new-generation environment-friendly diluent PU-10, and the mixing amount of the diluent accounts for 5-15% of the sum of the mass of the isocyanate, the mass of the polyethylene glycol and the mass of the cross-linking agent.
Further, in the step 4, the phase-change ceramsite is added into the polyurethane system for 5-10 s and then taken out, and the temperature is kept at 40-45 ℃ for 5-10 h, so that the polyurethane system on the phase-change ceramsite is primarily cured.
Further, in the step 5, the primarily cured phase-change ceramsite is placed in an oven with the temperature of 80-100 ℃, heated for 8-10 hours, taken out, and screened to obtain the phase-change aggregate.
Further, the preparation method of the phase-change ceramsite comprises the following steps:
step a: heating and melting polyethylene glycol at 120-170 ℃ to enable the polyethylene glycol to be in a flowing state;
step b: adding absolute ethyl alcohol into the polyethylene glycol melted in the step a for dilution, and reducing the viscosity of the polyethylene glycol;
step c: b, adding ceramsite into the polyethylene glycol in the step b, and stirring until the ceramsite is uniformly dispersed; wherein the mass ratio of the polyethylene glycol to the ceramsite is 5: 1-10: 1;
step d: and c, placing the system obtained in the step c in a vacuum drying oven, and keeping the system in a vacuum environment at the temperature of 120-190 ℃ for 0.5-5 h to enable the pores inside the ceramsite to fully adsorb the polyethylene glycol, so as to obtain the phase-change ceramsite.
Compared with the prior art, the invention has at least the following beneficial effects: the invention relates to a phase change aggregate for self-sensing and self-cooling of an asphalt pavement, which comprises phase change ceramsite and an encapsulation layer coated on the phase change ceramsite; the encapsulation layer comprises the following components: the graphene oxide coating comprises polyethylene glycol, a cross-linking agent, isocyanate and graphene oxide, wherein the mass of the graphene oxide accounts for 1-5% of the total mass of the polyethylene glycol, the cross-linking agent and the isocyanate; of polyethylene glycol, crosslinking agent and isocyanate, [ NCO ]: the molar ratio of [ OH ] is 1.1 to 1.3, and in the crosslinking agent, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4-0.7. According to the invention, the raw materials and the synthesis formula of the polyurethane packaging layer of the phase-change aggregate suitable for the asphalt pavement are strictly selected, and the graphene oxide containing rich hydroxyl groups is introduced into the polyurethane system through a chemical reaction, so that the dispersibility and the chemical stability of the graphene oxide in the polyurethane system are obviously improved, the thermal conductivity of the phase-change aggregate is fundamentally improved, the limitation on the thickness of the polyurethane packaging layer is reduced, and the preparation difficulty of the phase-change aggregate is greatly reduced.
Compared with the prior art, the preparation method of the phase change aggregate for self-perception and self-cooling of the asphalt pavement has the following advantages: the packaging material adopted by the prior art has no phase change function and low thermal conductivity coefficient, so that the thickness of the packaging layer is determined to be as small as possible on the premise of meeting the requirements on strength and hardness, and the phase change and heat storage function of polyethylene glycol in the ceramsite is ensured to be exerted. However, in the process of packaging the phase-change ceramsite, the thickness of the packaging layer is difficult to quantify, which undoubtedly increases the difficulty of the packaging process. Therefore, the polyurethane with the phase change function is prepared to encapsulate the phase change ceramsite, the raw materials and the synthesis formula of the polyurethane encapsulation layer of the phase change aggregate suitable for the asphalt pavement are strictly selected, and the graphene oxide containing rich hydroxyl groups is introduced into a polyurethane system through a chemical reaction, so that the dispersibility and the chemical stability of the graphene oxide in the polyurethane system are obviously improved, the thermal conductivity of the phase change aggregate is fundamentally improved, the limitation on the thickness of the polyurethane encapsulation layer is reduced, and the preparation difficulty of the phase change aggregate is greatly reduced; the phase-change aggregate obtained by the synthesis method and the formula not only prevents the phase-change substance from seeping out of the ceramsite when the phase-change substance is melted, but also remarkably improves the heat storage capacity of the phase-change aggregate, and further improves the regulation and control capacity on the temperature of the asphalt pavement; meanwhile, the strength of the polyurethane packaging layer is reduced in the high-temperature phase change process, and the polyurethane packaging layer synthesized by the self-made formula has higher strength and hardness; in addition, the thickness of the polyurethane packaging layer is not limited, the strength of the phase change aggregate is improved by increasing the thickness of the packaging layer, the damage resistance under the load action of the phase change aggregate is improved, and the durability of the packaging layer is further improved.
Further, in step 3, a diluent is added, and the thickness of the packaging layer is adjusted by reducing the overall viscosity of the polyurethane and prolonging the curing time, so as to achieve the purpose of perfect packaging.
Further, in the step 4, the phase-change ceramsite is added into the polyurethane system for 5-10 s and then taken out, and the temperature is kept at 40-45 ℃ for 5-10 h, so that the polyurethane system on the phase-change ceramsite is primarily cured to form the packaging strength.
Further, in the step 5, the primarily cured phase-change ceramsite is placed in an oven with the temperature of 80-100 ℃, heated for 8-10 hours, taken out, and screened, so that the phase-change aggregate with high strength and hardness can be obtained.
Furthermore, the preparation process of the phase-change ceramsite is easy to implement, and polyethylene glycol can be completely adsorbed in the open pores inside the ceramsite, so that the phase-change ceramsite is endowed with the maximum phase-change heat storage capacity.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a phase change aggregate for self-sensing and self-cooling of an asphalt pavement, which comprises phase change ceramsite and an encapsulation layer coated on the phase change ceramsite; wherein the encapsulation layer comprises the following components: polyethylene glycol, a cross-linking agent, isocyanate and graphene oxide. Specifically, the relative molecular weight of polyethylene glycol is one or more of 4000-10000; preferably, the crosslinking agent is a trifunctional glycerol; the isocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethyl diisocyanate.
The proportion of each component of the packaging layer is as follows: the mass of the graphene oxide accounts for 1-5% of the total mass of the polyethylene glycol, the cross-linking agent and the isocyanate.
In the polyethylene glycol, the crosslinking agent and the isocyanate, the ratio of the amount of [ NCO ] in the isocyanate to the sum of the amounts of [ OH ] in the polyethylene glycol and [ OH ] in the crosslinking agent is 1.1-1.3, and the ratio of the amount of [ OH ] in the crosslinking agent to the amount of [ OH ] in the polyethylene glycol is 0.4-0.7; that is, [ NCO ]: the molar ratio of [ OH ] is 1.1 to 1.3, and in the crosslinking agent, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4-0.7.
The embodiment of the preparation method of the phase change aggregate for self-sensing and self-cooling of the asphalt pavement comprises vacuum impregnation and physical coating, wherein the phase change aggregate is prepared by adopting the vacuum impregnation, and the phase change aggregate is packaged by adopting the physical coating.
Example 1
Polyethylene glycol 4000, glycerol, hexamethyl diisocyanate and graphene oxide are selected, and in the components, the molar ratio of [ NCO ]/[ OH ] is 1.2, wherein in the glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4, and the mass fraction of the graphene oxide is 2.5%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating and melting 100g of polyethylene glycol 4000 at 140 ℃ to make the polyethylene glycol in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 17g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 6: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 150 ℃ for 5 hours to ensure that the pores inside the ceramsite fully adsorb the polyethylene glycol to obtain the phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 4000 is heated to a molten state at 80 ℃;
step six: adding 0.62g of glycerol and 2.70g of graphene oxide into polyethylene glycol 4000 in a molten state, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 7.07g of hexamethyl diisocyanate and 8.62g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 8min at 80 ℃, reacting to obtain a polyurethane system, and then cooling to 45 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 5s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 40 ℃ for 7h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in a drying oven at 90 ℃ for 8 hours, taking out the phase change ceramsite to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 20% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 53.2 ℃, and the highest temperature reduction amplitude is more than 5 ℃.
Example 2
Polyethylene glycol 6000, glycerol, diphenylmethane diisocyanate and graphene oxide are selected, and in the components, the molar ratio of [ NCO ]/[ OH ] is 1.1, wherein in the glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.4, and the mass fraction of the graphene oxide is 1.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating and melting 100g of polyethylene glycol 6000 at 150 ℃ to make the polyethylene glycol 6000 in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 13g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 8: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 140 ℃ for 5 hours to ensure that the pores inside the ceramsite fully adsorb the polyethylene glycol to obtain the phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 6000 is heated to a molten state at 70 ℃;
step six: adding 0.41g of glycerol and 1.07g of graphene oxide into polyethylene glycol 6000 in a molten state, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 6.48g of diphenylmethane diisocyanate and 5.35g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 5min at 90 ℃, reacting to obtain a polyurethane system, and then cooling to 45 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 5s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 43 ℃ for 8h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) placing the primarily cured phase change ceramsite in the step eight in an oven with the temperature of 80-100 ℃, heating for 8-10 hours, taking out to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 30% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 55.3 ℃, and the highest temperature reduction amplitude is more than 5.5 ℃.
Example 3
Polyethylene glycol 4000, glycerol, diphenylmethane diisocyanate and graphene oxide are selected, wherein in the components, the molar ratio of [ NCO ]/[ OH ] is 1.3, wherein in the glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.6, and the mass fraction of the graphene oxide is 4.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating and melting 100g of polyethylene glycol 4000 at 130 ℃ to make the polyethylene glycol in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 20g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 5: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 180 ℃ for 1h to ensure that polyethylene glycol is fully adsorbed in pores inside the ceramsite to obtain phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 4000 is heated to a molten state at 80 ℃;
step six: adding 0.93g of glycerol and 4.39g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 8.75g of diphenylmethane diisocyanate and 16.45g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 6min at 90 ℃, reacting to obtain a polyurethane system, and then cooling to 45 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 10s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 45 ℃ for 5h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in a drying oven at 100 ℃ for 9 hours, taking out the phase change ceramsite to obtain phase change aggregate, performing secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by 5 percent; the phase-change aggregate replaces 20% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature of 54.7 ℃, and the highest temperature reduction amplitude can reach more than 4.5 ℃.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 30% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 53.7 ℃, and the highest temperature reduction amplitude is more than 5.5 ℃.
Example 4
Selecting polyethylene glycol 8000, glycerol, diphenylmethane diisocyanate and graphene oxide, wherein in the components, the molar ratio of [ NCO ]/[ OH ] is 1.3, wherein in the glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.5, and the mass fraction of the graphene oxide is 5.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating and melting 100g of polyethylene glycol 8000 at 170 deg.C to make it in a fluid state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 17g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 6: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 120 ℃ for 3 hours to ensure that the pores inside the ceramsite fully adsorb the polyethylene glycol to obtain the phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 8000 is heated to a molten state at 90 ℃;
step six: adding 0.39g of glycerol and 5.23g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 4.10g of diphenylmethane diisocyanate and 12.54g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 10min at 70 ℃, reacting to obtain a polyurethane system, and then cooling to 50 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 8s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 40 ℃ for 10h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in a 70 ℃ drying oven for 8 hours, taking out the phase change ceramsite to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 30% of fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 56.8 ℃, and the highest temperature reduction range is more than 5 ℃.
Example 5
Selecting polyethylene glycol 2000, glycerol, isophorone diisocyanate and graphene oxide, wherein the molar ratio of [ NCO ]/[ OH ] in the components is 1.2, wherein [ OH ] in the glycerol: the molar ratio of [ OH ] in the polyethylene glycol is 0.5, and the mass fraction of the graphene oxide is 3.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating 100g of polyethylene glycol 2000 at 120 ℃ to melt the polyethylene glycol 2000 so that the polyethylene glycol is in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 10g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 10: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 160 ℃ for 0.5h to ensure that the pores inside the ceramsite fully adsorb the polyethylene glycol to obtain the phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 2000 is heated to a molten state at 70 ℃;
step six: adding 1.54g of glycerol and 3.65g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 20.01g of isophorone diisocyanate and 12.16g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 10min at 80 ℃, reacting to obtain a polyurethane system, and then cooling to 45 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 7s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 43 ℃ for 7h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in an oven at 80 ℃ for 10 hours, taking out the phase change ceramsite to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 30% of fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 45.4 ℃, and the highest temperature reduction amplitude is more than 5 ℃.
Example 6
Polyethylene glycol 6000, trimethylolpropane, toluene diisocyanate and graphene oxide are selected, and in the components, the molar ratio of [ NCO ]/[ OH ] is 1.2, wherein in glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.5, and the mass fraction of the graphene oxide is 1.5%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: 100g of polyethylene glycol 2000 was melted by heating at 130 ℃ to be in a fluid state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 14.5g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 7: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 120 ℃ for 4 hours to ensure that the pores inside the ceramsite fully adsorb the polyethylene glycol to obtain the phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 6000 is heated to a molten state at 90 ℃;
step six: adding 0.90g of trimethylolpropane and 1.60g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 5.11g of toluene diisocyanate and 7.42g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 9min at 70 ℃, reacting to obtain a polyurethane system, and then cooling to 47 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 10s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 40 ℃ for 7h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in a drying oven at 90 ℃ for 10 hours, taking out the phase change ceramsite to obtain phase change aggregate, performing secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 20% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 55.5 ℃, and the highest temperature reduction amplitude is more than 5 ℃.
Example 7
Polyethylene glycol 8000, trimethylolpropane, hexamethyldiisocyanate and graphene oxide are selected, and in the components, the molar ratio of [ NCO ]/[ OH ] is 1.3, wherein in glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.7, and the mass fraction of the graphene oxide is 3.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating 100g of polyethylene glycol 2000 at 120 ℃ to melt the polyethylene glycol 2000 so that the polyethylene glycol is in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 20g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 5: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping for 3 hours in a vacuum environment at 190 ℃ to ensure that polyethylene glycol is fully adsorbed in pores inside the ceramsite to obtain phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 8000 is heated to a molten state at 70 ℃;
step six: adding 0.79g of trimethylolpropane and 1.60g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 3.16g of hexamethyl diisocyanate and 15.82g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 7min at 85 ℃, reacting to obtain a polyurethane system, and then cooling to 50 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 5s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 45 ℃ for 8h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in a drying oven at 90 ℃ for 8 hours, taking out the phase change ceramsite to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 20% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 56.9 ℃, and the highest temperature reduction amplitude is more than 5 ℃.
Example 8
Polyethylene glycol 4000, trimethylolethane, hexamethyldiisocyanate and graphene oxide are selected, and in the components, the molar ratio of [ NCO ]/[ OH ] is 1.2, wherein in glycerol, [ OH ]: the molar ratio of [ OH ] in the polyethylene glycol is 0.7, and the mass fraction of the graphene oxide is 2.0%. The preparation method comprises the following steps:
firstly, preparing phase-change ceramsite by vacuum impregnation, wherein the preparation method comprises the following steps:
the method comprises the following steps: heating and melting 100g of polyethylene glycol 4000 at 150 ℃ to make the polyethylene glycol in a flowing state;
step two: adding absolute ethyl alcohol into the polyethylene glycol melted in the step one to dilute, and reducing the viscosity of the polyethylene glycol;
step three: adding 14.5g of ceramsite into the polyethylene glycol obtained in the step two, and stirring until the ceramsite is uniformly dispersed;
respectively carrying out shelling, crushing and screening on the ceramsite before use to obtain the ceramsite with the particle size range of 0.15-2 mm; wherein the mass ratio of the polyethylene glycol to the ceramsite is 7: 1;
step four: placing the system obtained in the third step in a vacuum drying oven, and keeping the system in a vacuum environment at 180 ℃ for 2.5 hours to enable the pores inside the ceramsite to fully adsorb polyethylene glycol, so as to obtain phase-change ceramsite;
then, the phase-change ceramsite is packaged by physical coating, and the steps are as follows:
step five: under the protection of nitrogen, 100g of polyethylene glycol 8000 is heated to a molten state at 90 ℃;
step six: adding 1.41g of trimethylolethane and 2.20g of graphene oxide into molten polyethylene glycol, and stirring or ultrasonically dispersing until the mixture is uniform to obtain a physical blending system containing hydroxyl to be reacted;
step seven: adding 8.58g of hexamethyl diisocyanate and 13.20g of new-generation environment-friendly diluent PU-10 into the system obtained in the sixth step, stirring for 8min at 70 ℃, reacting to obtain a polyurethane system, and then cooling to 45 ℃;
step eight: completely immersing the phase-change ceramsite obtained in the step four into the polyurethane system obtained in the step seven for 8s, then taking out the phase-change ceramsite, and keeping the phase-change ceramsite adhered with the polyurethane system at 40 ℃ for 10h to preliminarily solidify the polyurethane system on the phase-change ceramsite;
step nine: and (5) heating the primarily cured phase change ceramsite in the step eight in an oven at 80 ℃ for 8 hours, taking out the phase change ceramsite to obtain phase change aggregate, carrying out secondary screening on the phase change aggregate, and collecting the phase change aggregate with the thickness of 0.3-2.36 mm.
The packaging process of the embodiment is simple; in the high-temperature phase change process, the polyurethane packaging layer always keeps enough hardness, and the leakage phenomenon does not occur; the mass loss rate of the packaged phase change aggregate after 80 times of thermal cycles is less than 2%, and the good thermal stability is embodied; compared with the traditional epoxy encapsulated phase change aggregate, the phase change latent heat of the phase change aggregate synthesized by the method is improved by more than 5%; the phase-change aggregate replaces 30% of the fine aggregate SMA-10 mixture, and the temperature reduction effect is gradually shown after the temperature is 53.6 ℃, and the highest temperature reduction amplitude is more than 5 ℃.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. A preparation method of phase change aggregate for self-sensing and self-cooling of asphalt pavement is characterized in that the phase change aggregate comprises phase change ceramsite and an encapsulation layer coated on the phase change ceramsite;
the packaging layer comprises the following components: the graphene oxide coating comprises polyethylene glycol, a cross-linking agent, isocyanate and graphene oxide, wherein the mass of the graphene oxide accounts for 1% -5% of the total mass of the polyethylene glycol, the cross-linking agent and the isocyanate; the cross-linking agent is trifunctional glycerol; the isocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethyl diisocyanate;
polyethylene glycol, crosslinking agent and isocyanate, -NCO: the molar ratio of-OH is 1.1-1.3, and in the cross-linking agent, the molar ratio of-OH: the molar ratio of-OH in the polyethylene glycol is 0.4-0.7;
the preparation method comprises the following steps:
step 1: heating the polyethylene glycol to a molten state;
step 2: adding the cross-linking agent and the graphene oxide into molten polyethylene glycol, and uniformly mixing to obtain a physical blending system containing hydroxyl to be reacted;
and step 3: adding the isocyanate and the diluent into the system obtained in the step 2, and reacting to obtain a polyurethane system;
and 4, step 4: adding the phase-change ceramsite into the polyurethane system obtained in the step (3), and taking out the phase-change ceramsite adhered with the polyurethane system to preliminarily cure the polyurethane system on the phase-change ceramsite;
and 5: drying the primarily cured phase-change ceramsite obtained in the step 4 to obtain phase-change aggregate;
the preparation method of the phase-change ceramsite comprises the following steps:
step a: heating and melting polyethylene glycol at 120-170 ℃ to enable the polyethylene glycol to be in a flowing state;
step b: adding absolute ethyl alcohol into the polyethylene glycol melted in the step a for dilution, and reducing the viscosity of the polyethylene glycol;
step c: b, adding ceramsite into the polyethylene glycol in the step b, and stirring until the ceramsite is uniformly dispersed; wherein the mass ratio of the polyethylene glycol to the ceramsite is 5: 1-10: 1;
step d: and C, placing the system obtained in the step C in a vacuum drying oven, and keeping the system at the temperature of 120-190 ℃ for 0.5-5 h to enable the pores inside the ceramsite to fully adsorb the polyethylene glycol, so as to obtain the phase-change ceramsite.
2. The preparation method of the phase change aggregate for self perception and self cooling of the asphalt pavement according to claim 1, wherein in the step 1, the heating temperature is 70-90 ℃ and the heating is carried out under the protection of inert gas; in the step 2, polyethylene glycol, a cross-linking agent and graphene oxide are uniformly mixed by stirring or ultrasonic dispersion.
3. The preparation method of the phase change aggregate for self perception and self cooling of the asphalt pavement according to claim 1, wherein in the step 3, the mixture is stirred for 5-10 min at 70-90 ℃, and then is cooled to 45-50 ℃; the diluent is an environment-friendly diluent PU-10, and the mixing amount of the diluent accounts for 5-15% of the sum of the mass of the isocyanate, the mass of the polyethylene glycol and the mass of the cross-linking agent.
4. The method for preparing the phase-change aggregate for self-perception and self-cooling of the asphalt pavement according to claim 1, wherein in the step 4, the phase-change ceramsite is added into the polyurethane system for 5-10 s, then taken out, and kept at 40-45 ℃ for 5-10 h, so that the polyurethane system on the phase-change ceramsite is primarily cured.
5. The preparation method of the phase change aggregate for self-perception and self-cooling of the asphalt pavement according to claim 1, wherein in the step 5, the primarily cured phase change ceramsite is placed in an oven at 80-100 ℃ to be heated for 8-10 hours, then taken out and screened to obtain the phase change aggregate.
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