WO2021135202A1 - 一种路用蓄能自发光环氧树脂混合料及其制备方法 - Google Patents

一种路用蓄能自发光环氧树脂混合料及其制备方法 Download PDF

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WO2021135202A1
WO2021135202A1 PCT/CN2020/105599 CN2020105599W WO2021135202A1 WO 2021135202 A1 WO2021135202 A1 WO 2021135202A1 CN 2020105599 W CN2020105599 W CN 2020105599W WO 2021135202 A1 WO2021135202 A1 WO 2021135202A1
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epoxy resin
stirring
phosphor
fine aggregate
luminous
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PCT/CN2020/105599
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English (en)
French (fr)
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蒋玮
周博
袁东东
肖晶晶
沙爱民
单金焕
卢灏
王沛
章庆
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长安大学
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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
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/14—Polyepoxides
    • E—FIXED CONSTRUCTIONS
    • E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
    • E01C7/00—Coherent pavings made in situ
    • E01C7/08—Coherent pavings made in situ made of road-metal and binders
    • E01C7/35—Toppings or surface dressings; Methods of mixing, impregnating, or spreading them
    • E01C7/358—Toppings or surface dressings; Methods of mixing, impregnating, or spreading them with a combination of two or more binders according to groups E01C7/351 - E01C7/356
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/80—Optical properties, e.g. transparency or reflexibility
    • C04B2111/807—Luminescent or fluorescent materials

Definitions

  • the invention belongs to the field of pavement engineering, and specifically relates to a road-use energy storage self-luminous epoxy resin mixture and a preparation method thereof.
  • Energy storage self-luminous pavement can be defined as a pavement material mixed with long afterglow powder, fluorescent stone and other fluorescent materials, which can absorb ultraviolet rays during the day to store energy, and emit fluorescence at night after the light disappears.
  • the realization of energy-storage self-luminous pavement is mainly achieved through two ways: (1), applying fluorescent coating on the surface of asphalt or cement pavement; (2) preparing fluorescent stone and mixing it into the pavement mixture.
  • both of these methods have certain limitations and deficiencies.
  • the present invention provides a road-use energy storage self-luminous epoxy resin mixture and a preparation method thereof, which have good luminous effect, long fluorescence time and excellent road performance.
  • a road-use energy storage self-luminous epoxy resin mixture comprising the following components: coarse aggregate, fine aggregate, epoxy resin, toughening agent, curing agent and phosphor;
  • the nominal particle size of the coarse aggregate is greater than 2.36 mm, the nominal particle size of the fine aggregate is 0.15 mm to 2.36 mm, and the nominal particle size of the phosphor is less than 0.15 mm;
  • the epoxy resin accounts for 6.0% to 10.0% of the total mass of the coarse aggregate and the fine aggregate
  • the toughening agent accounts for 0.4% to 1.0% of the total mass of the coarse aggregate and the fine aggregate %
  • the curing agent accounts for 1.0% to 2.5% of the total mass of the coarse aggregate and the fine aggregate
  • the phosphor accounts for 5.0% to 10.0 of the total mass of the coarse aggregate and the fine aggregate %.
  • the coarse aggregate is basalt or diabase.
  • the fine aggregate is limestone, diabase or gneiss.
  • the epoxy resin adopts bisphenol A diglycidyl ether E51 type epoxy resin or E44 type epoxy resin.
  • the toughening agent adopts dibutyl phthalate toughening agent.
  • the curing agent adopts 593 curing agent or polyetheramine D-230 curing agent.
  • the phosphor adopts a long afterglow material, and the afterglow visible time is longer than 8h.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Add the toughening agent to the epoxy resin, stir and mix evenly;
  • Step 2 Add the curing agent to the mixture obtained in Step 1, stir and mix uniformly to obtain an adhesive;
  • Step 3 Add the phosphor to the adhesive obtained in step 2, stir and mix uniformly to obtain a phosphor cement;
  • Step 4 Add the phosphor binder obtained in step 3 to the fine aggregate, stir and mix uniformly, add the coarse aggregate, stir and mix uniformly, to obtain an energy storage self-luminous epoxy resin mixture.
  • step 1 the stirring temperature is 25°C-30°C, the stirring speed is 1500r/min, and the stirring time is 10-15min;
  • step 2 the stirring temperature is 25°C-30°C, the stirring speed is 2000r/min, and the stirring time is 10-15min;
  • step 3 the time of the adding process is 3-5min, and the emulsifying shearer is used for stirring, the stirring temperature is 25°C-30°C, the stirring speed is 4000r/min, and the stirring time is 15-20min;
  • step 4 the stirring temperature of the phosphor binder and the fine aggregate is 25°C-30°C, and the stirring time is 3-5min; after adding the coarse aggregate, the stirring temperature is 25°C-30°C, The stirring time is 3-5min.
  • a road-use energy storage self-luminous epoxy resin mixture of the present invention includes the following components: coarse aggregate, fine aggregate, epoxy resin, and Toughener, curing agent and phosphor; the nominal particle size of coarse aggregate is greater than 2.36mm, the nominal particle size of fine aggregate is 0.15mm ⁇ 2.36mm, the nominal particle size of phosphor is less than 0.15mm; epoxy resin accounts for coarse aggregate 6.0% ⁇ 10.0% of the total mass of aggregates and fine aggregates, toughening agent accounts for 0.4% ⁇ 1.0% of the total mass of coarse aggregates and fine aggregates, and curing agent accounts for 1.0% ⁇ 1.0% of the total mass of coarse aggregates and fine aggregates.
  • the phosphor accounts for 5.0% to 10.0% of the total mass of the coarse aggregate and the fine aggregate.
  • the resin binder formed by selecting the above components and mixing according to the above ratio has good viscosity and fluidity, and is convenient for construction; at the same time, the cured resin has high strength and can meet the requirements of road performance.
  • the resin can wrap the phosphor well, protect the phosphor from external factors (water, tire wear, etc.), fully protect the phosphor's luminous performance, high compressive strength, and high temperature resistance to rutting. Good, strong low temperature deformation ability, improve the service life of self-luminous pavement.
  • the invention uses colorless and transparent epoxy resin to skillfully exert the advantages of phosphors, so that the epoxy resin mixture has good light transmittance and ideal luminous effect.
  • the epoxy resin ratio can meet the requirements of road performance and fluorescence Powder has a protective effect; the use of fluorescent powder with a nominal particle size of less than 0.15mm replaces the fine aggregate less than 0.15mm, which does not affect the mechanical properties of the pavement structure, and has the beneficial effect of energy storage and luminescence.
  • the coarse aggregate adopts basalt or diabase, which has strong compressive resistance, low crushing value, strong corrosion resistance, abrasion resistance, good angularity, and strong compaction between particles. It is a highway The best choice for paving coarse aggregates.
  • the fine aggregate is limestone, diabase or gneiss, which has the advantages of strong corrosion resistance and wear resistance, and is the best choice for road paving fine aggregate.
  • the epoxy resin adopts bisphenol A diglycidyl ether E51 type epoxy resin or E44 type epoxy resin.
  • This type of epoxy resin has strong adhesion, low viscosity, high toughness, low shrinkage and superior mechanical properties. It has the characteristics of chemical resistance and heat resistance. At the same time, it has a colorless and transparent appearance after curing, which is very beneficial to the phosphor luminescence and light excitation.
  • the toughening agent adopts dibutyl phthalate toughening agent.
  • the addition of this toughening agent to the epoxy resin can significantly increase the flexibility of the resin after curing, and improve its tensile and fatigue resistance properties. Good service for the pavement.
  • the curing agent adopts 593 curing agent or polyetheramine D-230 curing agent.
  • the curing agent is liquid at room temperature, which is convenient for operation, and has simple curing conditions. It can be cured quickly at room temperature, and the strength of the resin after curing is high. It has high hardness and is a colorless and transparent solid, which is very beneficial to the luminescence and light excitation of phosphors.
  • the phosphor adopts a long afterglow material, the visible time of afterglow is longer than 8h, and the long afterglow time can enable the self-luminous road surface to keep glowing overnight, which is beneficial to reduce the danger caused by lack of sight when driving at night.
  • the invention provides a method for preparing a road-use energy storage self-luminous epoxy resin mixture.
  • the mixture of epoxy resin and toughening agent is prepared under the conditions of temperature, agitating time and agitating speed defined by the present invention, which fully meets the requirements The requirements of epoxy resin road performance, and ensure the feasibility of operation, provide a stable basis for the preparation of epoxy resin mixture; under the conditions of limited temperature, limited stirring time and limited stirring speed, the curing agent
  • the adhesive is prepared by adding epoxy resin and toughening agent in a limited ratio to ensure that the adhesive has excellent viscosity, stable performance, and strong operability; at limited temperature, limited mixing time and limited
  • the phosphor cement is prepared under the condition of the stirring speed to ensure the excellent performance of the phosphor cement, and the emulsification shearing machine is used to ensure the uniform stability of the phosphor cement; by controlling the order of adding fine aggregate and coarse aggregate , To ensure that the aggregate and phosphor cementing material form a stable and reliable glue, the mixing time and mixing temperature are easily control
  • the road-use energy-storing self-luminous epoxy resin mixture of the present invention is laid on the road surface.
  • the road surface has good luminous effect and high intensity.
  • the resin can well protect the phosphor, has long service life, low maintenance cost, and is very good. This makes up for the lack of the existing luminescent coating technology that is easily affected by external factors and reduces the luminous effect, and at the same time avoids the disadvantage of insufficient luminous intensity caused by the use of luminescent stones to pave the road.
  • the invention effectively solves the hidden safety hazards of rural roads at night, and provides a solution for the construction of intelligent roads; the raw materials of the energy storage self-luminous epoxy resin mixture for the roads of the invention are economical and reasonable, have good luminous effects and strong operability It can be widely used in rural roads or road structures lacking lighting facilities in the urban-rural junction, which is of great significance.
  • Fig. 1 is a flow chart of a method for preparing a road-use energy storage self-luminous epoxy resin mixture of the present invention.
  • the energy storage self-luminous epoxy resin mixture for road use of the present invention includes the following components: coarse aggregate, fine aggregate, epoxy resin, toughening agent, curing agent and fluorescent powder.
  • Coarse aggregate and fine aggregate are designed in accordance with the current specification "Technical Specification for Highway Asphalt Pavement Construction” (JTG F40-2004) design gradation.
  • the gradation is suitable for ordinary dense gradation asphalt mixture, porous asphalt mixture, and asphalt mastic. Gravel etc.
  • the nominal particle size of the coarse aggregate is greater than 2.36mm.
  • the coarse aggregate adopts basalt or diabase stone with good lithology, low needle-like content and good angularity; the nominal particle size of the fine aggregate is 0.15mm ⁇ 2.36mm, The fine aggregate is limestone, diabase or gneiss; the nominal particle size of the phosphor is less than 0.15mm.
  • Epoxy resin accounts for 6.0% to 10.0% of the total mass of coarse and fine aggregates
  • toughening agent accounts for 0.4% to 1.0% of the total mass of coarse and fine aggregates
  • curing agent accounts for coarse and fine aggregates. 1.0% to 2.5% of the total mass
  • the phosphor occupies 5.0% to 10.0% of the total mass of the coarse aggregate and the fine aggregate.
  • the epoxy resin adopts bisphenol A diglycidyl ether E51 type epoxy resin or E44 type epoxy resin; the toughening agent adopts dibutyl phthalate toughening agent, and the epoxy resin is colorless, transparent and light-transmitting.
  • the advantages of good light-emitting effect, and epoxy resin wraps the phosphor, which effectively protects the phosphor;
  • the curing agent adopts 593 curing agent or polyether formed by the addition of diethylene triamine and butyl glycidyl ether Amine D-230 curing agent, the curing agent is colorless and transparent, has the advantages of good light transmission, and ideal luminous effect;
  • the phosphor adopts aluminate-based or silicate-based long afterglow materials excited by rare earth ions europium and dysprosium, It mainly plays the role of energy storage and luminescence.
  • the afterglow visible time is longer than 8h.
  • the afterglow visible time refers to the time from when the sample is excited to the brightness decays to 0.32mcd/m 2 .
  • Long afterglow luminescent material is abbreviated as long afterglow material. It is a kind of light-induced light that emits visible light when excited by a light source and stores part of the light energy obtained. After the excitation is stopped, the energy is slowly released in the form of light. Luminescent material.
  • the preparation method of a road-use energy storage self-luminous epoxy resin mixture of the present invention includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction” ⁇ (JTG F40-2004) Carry out gradation design;
  • Step 2 Weigh the epoxy resin and toughener according to the design gradation by weight percentage.
  • the content of toughener is 0.4%-1.0% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate. 6.0%-10.0% of the total mass of materials and fine aggregates, add the toughening agent to the epoxy resin, keep stirring during the addition process, and stir through a stirrer. The temperature during stirring is maintained at 25°C-30°C, and the stirring speed is 1500r /min, the stirring time is 10-15min, to obtain mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 1.0%-2.5% of the total mass of the coarse aggregate and the fine aggregate.
  • the curing agent is added to the mixture of epoxy resin and toughening agent A In the process of adding, keep stirring continuously, and stir through a stirrer. During stirring, the temperature is maintained at 25°C-30°C, the stirring speed is 2000r/min, and the stirring time is 10-15min to obtain adhesive B;
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 5%-10% of the total mass of the coarse aggregate and the fine aggregate.
  • Add the phosphor to the adhesive B, and the adding process time is 3 -5min, keep stirring continuously during the adding process, stir through the emulsifying shearing machine, keep the temperature at 25°C-30°C during stirring, the stirring speed is 4000r/min, and the stirring time is 15-20min, to obtain the phosphor cement C;
  • Step 5 Add phosphor cement C to the fine aggregate. After the addition is complete, use a stirring pot to stir. During stirring, keep the temperature at 25°C-30°C, and the stirring time is 3-5min. Phosphor cement C and fine aggregate After the stirring is completed, the coarse aggregate is added, and after the addition is completed, a stirring pot is used for stirring, and the temperature is maintained at 25°C-30°C during stirring, and the stirring time is 3-5min to obtain an energy-storing self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out gradation design, the gradation design is shown in Table 1.
  • Step 2 Weigh the epoxy resin and toughening agent according to the design grade in Table 1 by weight percentage.
  • the content of toughening agent is 0.4% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate. And 7.0% of the total mass of the fine aggregate, add the toughening agent to the epoxy resin, keep stirring during the addition process, and stir through the stirrer. The temperature is maintained at 25°C during stirring, the stirring speed is 1500r/min, and the stirring time is 10min.
  • Get mixture A
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 1.2% of the total mass of the coarse aggregate and the fine aggregate.
  • the curing agent is added to the mixture A of epoxy resin and toughening agent, and added The process keeps stirring continuously, and stirs through a stirrer. During stirring, the temperature is maintained at 25°C, the stirring speed is 2000r/min, and the stirring time is 10min to obtain adhesive B;
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 6% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process time is 3 minutes, and the adding process Keep stirring continuously, and stir through an emulsifying shearing machine. During stirring, the temperature is maintained at 25°C, the stirring speed is 4000r/min, and the stirring time is 15min to obtain phosphor cement C;
  • Step 5 Add the phosphor binder C to the fine aggregate. After the addition is complete, use a stirring pot to stir. During stirring, keep the temperature at 25°C and the stirring time for 3 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is completed, use a stirring pot to stir, the temperature is maintained at 25°C during stirring, and the stirring time is 3 minutes to obtain an energy-storing self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out the gradation design.
  • the gradation design is shown in Table 2.
  • Step 2 Weigh the epoxy resin and toughening agent according to the design grade in Table 1 by weight percentage.
  • the content of toughening agent is 0.4% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate.
  • 8% of the total mass of the fine aggregate add the toughening agent to the epoxy resin, keep stirring continuously during the adding process, stir through the stirrer, keep the temperature at 26°C during stirring, the stirring speed is 1500r/min, and the stirring time is 11min , Get mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 1.0% of the total mass of the coarse aggregate and the fine aggregate.
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 8% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process time is 4 minutes, and the adding process Keep stirring continuously, and stir through the emulsifying shearing machine. During stirring, the temperature is maintained at 26°C, the stirring speed is 4000r/min, and the stirring time is 16min to obtain phosphor cement C;
  • Step 5 Add the phosphor binder C to the fine aggregate. After the addition is complete, use a stirring pot to stir. Keep the temperature at 26°C during stirring, and the stirring time is 4 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is complete, use a stirring pot to stir, the temperature is maintained at 26°C during stirring, and the stirring time is 3 minutes to obtain the energy-storing self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out gradation design, the gradation design is shown in Table 3.
  • Step 2 Weigh the epoxy resin and toughening agent according to the design grade in Table 1 by weight percentage, the content of toughening agent is 0.6% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate And 10.0% of the total mass of the fine aggregate, add the toughening agent to the epoxy resin, keep stirring during the addition process, and stir through the stirrer. The temperature is kept at 28°C during stirring, the stirring speed is 1500r/min, and the stirring time is 12min. , Get mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 2.5% of the total mass of the coarse aggregate and the fine aggregate.
  • Step 4 Weigh the phosphor according to the design gradation by weight percentage.
  • the phosphor mass is 10% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process takes 5 minutes.
  • the adding process Keep stirring continuously, and stir through the emulsifying shearing machine. During stirring, the temperature is kept at 28°C, the stirring speed is 4000r/min, and the stirring time is 18min to obtain phosphor cement C;
  • Step 5 Add the phosphor binder C to the fine aggregate. After the addition is complete, use a stirring pot to stir. Keep the temperature at 28°C during stirring, and the stirring time is 5 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is completed, use a stirring pot to stir, the temperature is maintained at 28°C during stirring, and the stirring time is 5 minutes to obtain the energy-storing self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out gradation design, the gradation design is shown in Table 4.
  • Step 2 Weigh the epoxy resin and toughening agent according to the design grade in Table 1 by weight percentage.
  • the content of toughening agent is 0.8% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate.
  • 6.0% of the total mass of the fine aggregate add the toughening agent to the epoxy resin, keep stirring during the adding process, and stir through the stirrer. The temperature is maintained at 30°C during stirring, the stirring speed is 1500r/min, and the stirring time is 15min. , Get mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 2.0% of the total mass of the coarse aggregate and the fine aggregate.
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 8.0% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process takes 3 minutes.
  • the adding process Keep stirring continuously, and stir through an emulsifying shearing machine. During stirring, the temperature is maintained at 30°C, the stirring speed is 4000r/min, and the stirring time is 20min to obtain phosphor cement C;
  • Step 5 Add phosphor binder C to the fine aggregate, stir with a stirring pot after the addition is complete, keep the temperature at 30°C during stirring, and stir for 3 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is completed, use a stirring pot to stir, the temperature is maintained at 30°C during stirring, and the stirring time is 3 minutes to obtain the energy storage self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out the gradation design.
  • the gradation design is shown in Table 5.
  • Step 2 Weigh the epoxy resin and toughening agent according to the design grade in Table 1 by weight percentage, the content of toughening agent is 1.0% of the total mass of coarse aggregate and fine aggregate, and the content of epoxy resin is coarse aggregate And 10.0% of the total mass of the fine aggregate, add the toughening agent to the epoxy resin, keep stirring during the addition process, and stir through the stirrer. The temperature is kept at 26°C during stirring, the stirring speed is 1500r/min, and the stirring time is 13min , Get mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 1.5% of the total mass of the coarse aggregate and the fine aggregate.
  • the curing agent is added to the mixture A of epoxy resin and toughening agent, and added The process keeps stirring continuously, and stirs with a stirrer. During stirring, the temperature is kept at 26°C, the stirring speed is 2000r/min, and the stirring time is 13min to obtain adhesive B;
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 5% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process time is 4 minutes, and the adding process Keep stirring continuously, and stir through the emulsifying shearing machine. During stirring, the temperature is kept at 26°C, the stirring speed is 4000r/min, and the stirring time is 18min to obtain phosphor cement C;
  • Step 5 Add the phosphor binder C to the fine aggregate. After the addition is complete, use a stirring pot to stir. Keep the temperature at 26°C during stirring, and the stirring time is 4 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is completed, use a stirring pot to stir, the temperature is maintained at 26°C during stirring, and the stirring time is 4 minutes to obtain an energy-storing self-luminous epoxy resin mixture.
  • a preparation method of energy storage self-luminous epoxy resin mixture for road use includes the following steps:
  • Step 1 Coarse aggregates (nominal particle size greater than 2.36mm), fine aggregates (nominal particle size 0.15mm ⁇ 2.36mm) and phosphors (nominal particle size less than 0.15mm) are in accordance with the current standard "Technical Specification for Highway Asphalt Pavement Construction" ⁇ (JTG F40-2004) Carry out the gradation design.
  • the gradation design is shown in Table 6.
  • Step 2 Weigh the epoxy resin and the toughening agent according to the design grade in Table 1 by weight percentage, the content of the toughening agent is 1.0% of the total mass of the coarse aggregate and the fine aggregate, and the content of the epoxy resin is the coarse aggregate And 6.0% of the total mass of the fine aggregate, add the toughening agent to the epoxy resin, keep stirring during the adding process, and stir through the stirrer. The temperature is kept at 29°C during stirring, the stirring speed is 1500r/min, and the stirring time is 14min. , Get mixture A;
  • Step 3 Weigh the curing agent by weight according to the design gradation.
  • the content of the curing agent is 1.0% of the total mass of the coarse aggregate and the fine aggregate.
  • Step 4 Weigh the phosphor according to the design gradation according to the weight percentage.
  • the phosphor mass is 9.0% of the total mass of the coarse aggregate and the fine aggregate.
  • the adding process takes 5 minutes.
  • the adding process Keep stirring continuously, and stir through an emulsifying shearing machine. During stirring, the temperature is maintained at 29°C, the stirring speed is 4000r/min, and the stirring time is 20min to obtain phosphor cement C;
  • Step 5 Add the phosphor binder C to the fine aggregate. After the addition is complete, use a stirring pot to stir. Keep the temperature at 29°C during stirring, and the stirring time is 5 minutes. After the phosphor binder C and the fine aggregate are stirred, add the coarse Aggregate, after the addition is completed, use a stirring pot to stir, the temperature is maintained at 29°C during stirring, and the stirring time is 5 minutes to obtain the energy-storing self-luminous epoxy resin mixture.

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Abstract

一种路用蓄能自发光环氧树脂混合料及其制备方法，包括如下组分：粗集料、细集料、环氧树脂、增韧剂、固化剂和荧光粉；粗集料的公称粒径大于2.36mm，细集料的公称粒径为0.15mm～2.36mm，荧光粉的公称粒径小于0.15mm；环氧树脂占粗集料和细集料总质量的6.0％～10.0％，增韧剂占粗集料和细集料总质量的0.4％～1.0％，固化剂占粗集料和细集料总质量的1.0％～2.5％，荧光粉占粗集料和细集料总质量的5.0％～10.0％。通过运用无色透明的环氧树脂巧妙地发挥了荧光粉的优点，使环氧树脂混合料透光性好，发光效果理想，环氧树脂配比可以满足路用性能的要求并对荧光粉起保护作用；采用公称粒径小于0.15mm的荧光粉替代了小于0.15mm的细集料，既不影响路面结构的力学性能，而且具有蓄能发光的有益效果。

Description

一种路用蓄能自发光环氧树脂混合料及其制备方法 技术领域
本发明属于路面工程领域，具体涉及一种路用蓄能自发光环氧树脂混合料及其制备方法。
背景技术
截止2018年底，我国农村公路总里程达到403.97万公里，农村公路线长面广，安装路侧照明设施成本高、耗时长，且消耗大量的电力资源，并造成强光污染，因此，我国农村公路夜间缺少照明设施，普通的标志标线必须有灯光照射才能反光，导致行人或非机动车辆无法及时清晰地看到标志标线而发生危险，同时给交通安全带来隐患。因此，开发蓄能自发光路面意义重大。
蓄能自发光路面可以定义为在路面材料中掺入长余辉粉、荧光石等荧光材料，白天可以吸收紫外线等进行蓄能，在夜晚光线消失后放出荧光的路面。现阶段，蓄能自发光路面的实现主要通过两种途径：(一)、在沥青或水泥路面表面涂刷荧光涂层；(二)、制备荧光石掺入路面混合料中。但是这两种方法都存在一定的局限与不足。在路面表面涂刷荧光涂层，严重破坏了路面的构造深度，降低了路面的抗滑性能，尤其是雨雪天气，对行车安全非常不利；此外，路面表面的涂层直接与轮胎接触，非常容易磨损，从而引起涂层剥落，导致发光效果不理想，这使后期养护维修成本较高；而且涂层直接经受太阳、冰雪、雨水等气候因素影响，容易发生老化，使得发光性能逐渐降低。在路面混合料中掺入荧光石会降低路面强度与承载能力；另外，荧光石的发光强度较弱，发光效果不理想。
因此，鉴于现有蓄能自发光路面材料与设计存在的不足与缺陷，有必要开发研究更加完善的蓄能自发光路面材料与设计方法。
发明内容
针对现有技术中的技术问题，本发明提供了一种路用蓄能自发光环氧树脂混合料及其制备方法，发光效果好，荧光时间长，路用性能优良。
为了解决上述技术问题，本发明通过以下技术方案予以实现：
一种路用蓄能自发光环氧树脂混合料，包括如下组分：粗集料、细集料、环氧树脂、增韧剂、固化剂和荧光粉；
所述粗集料的公称粒径大于2.36mm，所述细集料的公称粒径为0.15mm～2.36mm，所述荧光粉的公称粒径小于0.15mm；
所述环氧树脂占所述粗集料和所述细集料总质量的6.0％～10.0％，所述增韧剂占所述粗集料和所述细集料总质量的0.4％～1.0％，所述固化剂占所述粗集料和所述细集料总质量的1.0％～2.5％，所述荧光粉占所述粗集料和所述细集料总质量的5.0％～10.0％。
进一步地，所述粗集料采用玄武岩或辉绿岩。
进一步地，所述细集料采用石灰岩、辉绿岩或片麻岩。
进一步地，所述环氧树脂采用双酚A二缩水甘油醚E51型环氧树脂或E44型环氧树脂。
进一步地，所述增韧剂采用邻苯二甲酸二丁酯增韧剂。
进一步地，所述固化剂采用593固化剂或聚醚胺类D-230固化剂。
进一步地，所述荧光粉采用长余辉材料，余辉可见时间大于8h。
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：将所述增韧剂加入所述环氧树脂中，搅拌混合均匀；
步骤2：将所述固化剂加入步骤1得到的混合物中，搅拌混合均匀得到胶黏剂；
步骤3：将所述荧光粉加入步骤2得到的所述胶黏剂中，搅拌混合均匀得到荧光粉胶结料；
步骤4：将步骤3得到的所述荧光粉胶结料加入所述细集料中，搅拌混合均匀后加入所述粗集料，搅拌混合均匀，得到蓄能自发光环氧树脂混合料。
进一步地，步骤1中，搅拌温度为25℃～30℃，搅拌转速为1500r/min，搅拌时间为10～15min；
步骤2中，搅拌温度为25℃-30℃，搅拌转速为2000r/min，搅拌时间为10-15min；
步骤3中，加入过程的时间为3-5min，采用乳化剪切机进行搅拌，搅拌温度为25℃-30℃，搅拌转速为4000r/min，搅拌时间为15-20min；
步骤4中，所述荧光粉胶结料与所述细集料的搅拌温度为25℃-30℃，搅拌时间为3-5min；加入所述粗集料后，搅拌温度为25℃-30℃，搅拌时间为3-5min。
与现有技术方案相比，本发明至少具有以下有益效果：本发明一种路用蓄能自发光环氧树脂混合料，包括如下组分：粗集料、细集料、环氧树脂、增韧剂、固化剂和荧光粉；粗集料的公称粒径大于2.36mm，细集料的公称粒径为0.15mm～2.36mm，荧光粉的公称粒径小于0.15mm；环氧树脂占粗集料和细集料总质量的6.0％～10.0％，增韧剂占粗集料和细集料总质量的0.4％～1.0％，固化剂占粗集料和细集料总质量的1.0％～2.5％，荧光粉占粗集料和细集料总质量的5.0％～10.0％。选择上述组分并按照上述比例拌和而成的树脂粘结剂具有很好的粘性与流动性，方便施工；同时固化后的树脂强度高，可满足路用性能要求。另外，树脂可以很好的对荧光粉进行了包裹，很好的保护荧光粉不受外界因素(水、轮胎磨耗等)影响，充分保护荧光粉的发光性能，抗压强度高，高温抗车辙性能好，低温变形能力强，提升自发光路面的使用寿命。本发明通过运用无色透明的环氧树脂巧妙地发挥了荧光粉的优点，使环氧树脂混合料透光性好，发光效果理想，环氧树脂配比可以满足路用性能的要求并对荧光粉其保护作用；采用公称粒径小于0.15mm的荧光粉替代了小于0.15mm的细集料，既不影响路面结构的力学性能，而且具有蓄能发光的有益效果。
进一步地，粗集料采用玄武岩或辉绿岩，该岩类具有抗压性强、压碎值低、抗腐蚀性强、耐磨、棱角性好，颗粒之间的嵌挤作用强，是公路铺筑粗集料的最佳选择。
进一步地，细集料采用石灰岩、辉绿岩或片麻岩，该岩类具有抗腐蚀性强、耐磨等优点， 是公路铺筑细集料的最优选择。
进一步地，环氧树脂采用双酚A二缩水甘油醚E51型环氧树脂或E44型环氧树脂，这类型环氧树脂有着附着力强、低粘度、韧性高、收缩力小，优越的机械性能和抗化学药品及耐热性等特点，同时，固化后有着无色透明的外观，对荧光粉发光和受光激发十分有利。
进一步地，增韧剂采用邻苯二甲酸二丁酯增韧剂，环氧树脂中加入该增韧剂可以显著的增加树脂固化后的柔韧性，提高其抗拉伸性能与抗疲劳性能，更好的为路面服务。
进一步地，固化剂采用593固化剂或聚醚胺类D-230固化剂，该固化剂常温呈液体，方便操作，且固化条件简易，常温就可很快的进行固化，同时树脂固化后强度高硬度大，呈无色透明固体，对荧光粉的发光与受光激发十分有利。
进一步地，荧光粉采用长余辉材料，余辉可见时间大于8h，余辉时间长可使得自发光路面能够维持一晚上发光，有利于减少夜间行车因视线不足引起的危险。
本发明一种路用蓄能自发光环氧树脂混合料的制备方法，在本发明限定的温度、限定的搅拌时间和限定的搅拌速度条件下制备环氧树脂与增韧剂的混合物，充分满足环氧树脂路用性能的要求，并且保证了操作的可行性，为环氧树脂混合料的制备提供了稳定的基础；在限定的温度、限定的搅拌时间和限定的搅拌速度条件下将固化剂按照限定的比例加入环氧树脂与增韧剂的混合物中制备胶黏剂，保证了胶黏剂具有优异的黏度，且性能稳定，可操作性强；在限定的温度、限定的搅拌时间和限定的搅拌速度条件下制备荧光粉胶结料，保证了荧光粉胶结料优异的使用性能，采用乳化剪切机保证了荧光粉胶结料的均匀稳定性；通过控制添加细集料和粗集料的顺序，保证了集料与荧光粉胶结料形成稳定可靠的胶浆，拌和时间和拌和温度均容易可控，优先保证了施工和易性。采用本发明方法制备的混合料固化后能够具备很好的抗压强度，同时发光效果也能够很好的发挥，满足使用要求。
将本发明的路用蓄能自发光环氧树脂混合料铺设于路面，该路面发光效果好，强度高，同 时树脂可以很好的对荧光粉进行保护，使用寿命长，维护成本低，很好的弥补了现有的发光涂层技术容易受到外界因素影响而降低发光效果的不足，同时避免了采用发光石铺筑道路引起的发光强度不足的劣势。本发明有效解决了农村公路夜间存在的安全隐患，为智能公路的建设提供了一种解决方案；本发明路用蓄能自发光环氧树脂混合料原材料经济合理，发光效果好，可操作性强，可广泛应用于农村公路或者城乡结合部缺少照明设施的道路结构中，具有重大意义。
为使本发明的上述目的、特征和优点能更明显易懂，下文特举较佳实施例，并配合所附附图，作详细说明如下。
附图说明
为了更清楚地说明本发明具体实施方式中的技术方案，下面将对本发明一种路用蓄能自发光环氧树脂混合料制备方法绘制制备流程图。
图1为本发明一种路用蓄能自发光环氧树脂混合料的制备方法的流程图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明一种路用蓄能自发光环氧树脂混合料，包括如下组分：粗集料、细集料、环氧树脂、增韧剂、固化剂和荧光粉。粗集料和细集料按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)设计级配进行设计，级配适用于普通密级配沥青混合料、多孔沥青混合料、沥青玛蹄脂碎石等。粗集料的公称粒径大于2.36mm，粗集料采用玄武岩或辉绿岩岩性好、针片状含量低、棱角性好的石料；细集料的公称粒径为0.15mm～2.36mm，细集料采用石灰岩、辉绿岩或片麻岩；荧光粉的公称粒径小于0.15mm。环氧树脂占粗集料和细集料总质量的6.0％～10.0％， 增韧剂占粗集料和细集料总质量的0.4％～1.0％，固化剂占粗集料和细集料总质量的1.0％～2.5％，荧光粉占粗集料和细集料总质量的5.0％～10.0％。
环氧树脂采用双酚A二缩水甘油醚E51型环氧树脂或E44型环氧树脂；增韧剂采用邻苯二甲酸二丁酯增韧剂，环氧树脂是无色透明、具有透光性好、发光效果理想的优点，且环氧树脂对荧光粉进行包裹，有效保护了荧光粉；固化剂采用二亚乙基三胺与丁基缩水甘油醚加成而成的593固化剂或聚醚胺类D-230固化剂，固化剂是无色透明、具有透光性好、发光效果理想的优点；荧光粉采用稀土离子铕和镝激发的铝酸盐基或者硅酸盐基长余辉材料，主要起蓄能发光作用，余辉可见时间大于8h，余辉可见时间是指将样品从被激发后到亮度衰减到0.32mcd/m 2的时间。长余辉发光材料简称长余辉材料，它是一类在光源激发下，发出可见光，并将获得的部分光能储存起来，在激发停止后，以光的形式将能量缓慢释放出来的一种光致发光材料。
本发明一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计；
步骤2：根据设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的0.4％-1.0％，环氧树脂掺量为粗集料和细集料总质量的6.0％-10.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持25℃-30℃，搅拌转速为1500r/min，搅拌时间为10-15min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的1.0％-2.5％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持25℃-30℃，搅拌转速为2000r/min，搅拌时间为10-15min， 得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的5％-10％，将荧光粉加入胶黏剂B中，加入过程时间为3-5min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持25℃-30℃，搅拌转速为4000r/min，搅拌时间为15-20min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持25℃-30℃，搅拌时间为3-5min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持25℃-30℃，搅拌时间为3-5min，得到一种蓄能自发光环氧树脂混合料。
遵从上述技术方案，提供如下实施例。
实施例1
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计，级配设计如表1所示。
表1
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 100 95 60 16 12 9 7 6 4
质量比(％) 0 5 35 44 4 3 2 1 2
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的0.4％，环氧树脂掺量为粗集料和细集料总质量的7.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持25℃，搅拌转速为 1500r/min，搅拌时间为10min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的1.2％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持25℃，搅拌转速为2000r/min，搅拌时间为10min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的6％，将荧光粉加入胶黏剂B中，加入过程时间为3min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持25℃，搅拌转速为4000r/min，搅拌时间为15min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持25℃，搅拌时间为3min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持25℃，搅拌时间为3min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为30.2MPa，余辉时间为8.5h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
实施例2
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计，级配设计如表2所示。
表2
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 100 95 60 44 32 23 14 8 5
质量比(％) 0 5 35 16 12 9 9 6 3
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的0.4％，环氧树脂掺量为粗集料和细集料总质量的8％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持26℃，搅拌转速为1500r/min，搅拌时间为11min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的1.0％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持26℃，搅拌转速为2000r/min，搅拌时间为11min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的8％，将荧光粉加入胶黏剂B中，加入过程时间为4min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持26℃，搅拌转速为4000r/min，搅拌时间为16min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持26℃，搅拌时间为4min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持26℃，搅拌时间为3min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为33.4MPa，余辉时间为9.0h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
实施例3
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计，级配设计如表3所示。
表3
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 95 62.5 27 20.5 19 16 11 10 8
质量比(％) 5 32.5 35.5 6.5 1.5 3 5 1 2
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的0.6％，环氧树脂掺量为粗集料和细集料总质量的10.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持28℃，搅拌转速为1500r/min，搅拌时间为12min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的2.5％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持28℃，搅拌转速为2000r/min，搅拌时间为12min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的10％，将荧光粉加入胶黏剂B中，加入过程时间为5min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持28℃，搅拌转速为4000r/min，搅拌时间为18min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持28℃，搅拌时间为5min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后 采用搅拌锅进行搅拌，搅拌时温度保持28℃，搅拌时间为5min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为41.6MPa，余辉时间为9.5h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
实施例4
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计，级配设计如表4所示。
表4
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 95 77 53 37 27 19 13 8 6
质量比(％) 5 18 24 16 10 8 6 5 2
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的0.8％，环氧树脂掺量为粗集料和细集料总质量的6.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持30℃，搅拌转速为1500r/min，搅拌时间为15min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的2.0％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持30℃，搅拌转速为2000r/min，搅拌时间为15min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的8.0％，将荧光粉加入胶黏剂B中，加入过程时间为3min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持30℃，搅拌转速为4000r/min，搅拌时间为20min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持30℃，搅拌时间为3min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持30℃，搅拌时间为3min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为31.9MPa，余辉时间为9.0h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
实施例5
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004)进行级配设计，级配设计如表5所示。
表5
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 95 65 21 16 12 10 7 5 4
质量比(％) 5 30 44 5 4 2 3 2 1
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和 细集料总质量的1.0％，环氧树脂掺量为粗集料和细集料总质量的10.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持26℃，搅拌转速为1500r/min，搅拌时间为13min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的1.5％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持26℃，搅拌转速为2000r/min，搅拌时间为13min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的5％，将荧光粉加入胶黏剂B中，加入过程时间为4min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持26℃，搅拌转速为4000r/min，搅拌时间为18min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持26℃，搅拌时间为4min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持26℃，搅拌时间为4min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为40.7MPa，余辉时间为8.2h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
实施例6
一种路用蓄能自发光环氧树脂混合料的制备方法，包括以下步骤：
步骤1：粗集料(公称粒径大于2.36mm)、细集料(公称粒径为0.15mm～2.36mm)和荧光粉(公称粒径小于0.15mm)按照现行规范《公路沥青路面施工技术规范》(JTG F40-2004) 进行级配设计，级配设计如表6所示。
表6
粒径(mm) 13.2 9.5 4.75 2.36 1.18 0.6 0.3 0.15 0.75
通过率(％) 100 95 44 26 20 17 14 9 8
质量比(％) 0 5 51 18 6 3 3 5 1
步骤2：根据表1设计级配按重量百分比称取环氧树脂和增韧剂，增韧剂掺量为粗集料和细集料总质量的1.0％，环氧树脂掺量为粗集料和细集料总质量的6.0％，将增韧剂加入环氧树脂中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持29℃，搅拌转速为1500r/min，搅拌时间为14min，得到混合物A；
步骤3：根据设计级配按重量百分比称取固化剂，固化剂掺量为粗集料和细集料总质量的1.0％，将固化剂加入环氧树脂与增韧剂的混合物A中，加入过程保持持续搅拌，通过搅拌器进行搅拌，搅拌时温度保持29℃，搅拌转速为2000r/min，搅拌时间为14min，得到胶黏剂B；
步骤4：根据设计级配按重量百分比称取荧光粉，荧光粉质量为粗集料和细集料总质量的9.0％，将荧光粉加入胶黏剂B中，加入过程时间为5min，加入过程保持持续搅拌，通过乳化剪切机进行搅拌，搅拌时温度保持29℃，搅拌转速为4000r/min，搅拌时间为20min，得到荧光粉胶结料C；
步骤5：将荧光粉胶结料C加入细集料中，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持29℃，搅拌时间为5min，荧光粉胶结料C与细集料搅拌完成后加入粗集料，加入完成后采用搅拌锅进行搅拌，搅拌时温度保持29℃，搅拌时间为5min，得到蓄能自发光环氧树脂混合料。
以抗压强度和余辉时间作为混合料性能的检验指标，采用室内试验检验通过上述制备方法制得的蓄能自发光环氧树脂混合料性能，得到蓄能自发光环氧树脂混合料的抗压强度为 29.9MPa，余辉时间为9.5h。可知通过该实施例制备得到的蓄能自发光环氧树脂混合料发光效果优异，固化后路面强度高，使用寿命长，能够满足使用要求。
最后应说明的是：以上所述实施例，仅为本发明的具体实施方式，用以说明本发明的技术方案，而非对其限制，本发明的保护范围并不局限于此，尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，其依然可以对前述实施例所记载的技术方案进行修改或可轻易想到变化，或者对其中部分技术特征进行等同替换；而这些修改、变化或者替换，并不使相应技术方案的本质脱离本发明实施例技术方案的精神和范围，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应所述以权利要求的保护范围为准。

Claims (9)

  1. 一种路用蓄能自发光环氧树脂混合料，其特征在于，包括如下组分：粗集料、细集料、环氧树脂、增韧剂、固化剂和荧光粉；
    所述粗集料的公称粒径大于2.36mm，所述细集料的公称粒径为0.15mm～2.36mm，所述荧光粉的公称粒径小于0.15mm；
    所述环氧树脂占所述粗集料和所述细集料总质量的6.0％～10.0％，所述增韧剂占所述粗集料和所述细集料总质量的0.4％～1.0％，所述固化剂占所述粗集料和所述细集料总质量的1.0％～2.5％，所述荧光粉占所述粗集料和所述细集料总质量的5.0％～10.0％。
  2. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述粗集料采用玄武岩或辉绿岩。
  3. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述细集料采用石灰岩、辉绿岩或片麻岩。
  4. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述环氧树脂采用双酚A二缩水甘油醚E51型环氧树脂或E44型环氧树脂。
  5. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述增韧剂采用邻苯二甲酸二丁酯增韧剂。
  6. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述固化剂采用593固化剂或聚醚胺类D-230固化剂。
  7. 根据权利要求1所述的一种路用蓄能自发光环氧树脂混合料，其特征在于，所述荧光粉采用长余辉材料，余辉可见时间大于8h。
  8. 根据权利要求1～7任一项所述的一种路用蓄能自发光环氧树脂混合料的制备方法，其特征在于，包括以下步骤：
    步骤1：将所述增韧剂加入所述环氧树脂中，搅拌混合均匀；
    步骤2：将所述固化剂加入步骤1得到的混合物中，搅拌混合均匀得到胶黏剂；
    步骤3：将所述荧光粉加入步骤2得到的所述胶黏剂中，搅拌混合均匀得到荧光粉胶结料；
    步骤4：将步骤3得到的所述荧光粉胶结料加入所述细集料中，搅拌混合均匀后加入所述粗集料，搅拌混合均匀，得到蓄能自发光环氧树脂混合料。
  9. 根据权利要求8所述的一种路用蓄能自发光环氧树脂混合料的制备方法，其特征在于：
    步骤1中，搅拌温度为25℃～30℃，搅拌转速为1500r/min，搅拌时间为10～15min；
    步骤2中，搅拌温度为25℃-30℃，搅拌转速为2000r/min，搅拌时间为10-15min；
    步骤3中，加入过程的时间为3-5min，采用乳化剪切机进行搅拌，搅拌温度为25℃-30℃，搅拌转速为4000r/min，搅拌时间为15-20min；
    步骤4中，所述荧光粉胶结料与所述细集料的搅拌温度为25℃-30℃，搅拌时间为3-5min；加入所述粗集料后，搅拌温度为25℃-30℃，搅拌时间为3-5min。
PCT/CN2020/105599 2020-01-02 2020-07-29 一种路用蓄能自发光环氧树脂混合料及其制备方法 WO2021135202A1 (zh)

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