Method for evaluating storage stability of cold-mixed epoxy asphalt
Analysis using fluorescence microscopy and Image Pro Plus software filled the gap in the evaluation of the storage stability of cold-mixed epoxy asphalt, enabling accurate assessment of its compatibility and stability, and ensuring the performance of the material in use.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- HOHAI UNIV
- Filing Date
- 2022-11-16
- Publication Date
- 2026-04-10
AI Technical Summary
The lack of an effective evaluation method for the storage stability of cold-mixed epoxy asphalt in the existing technology leads to segregation problems that seriously affect its performance.
A method for evaluating the storage stability of cold-mixed epoxy asphalt is provided, including sample preparation, storage placement, qualitative and quantitative evaluation steps. The method involves observing the phase distribution using a fluorescence microscope and analyzing the particle size distribution using Image Pro Plus software, and evaluating the storage stability by combining density difference values.
It enables qualitative and quantitative evaluation of the storage stability of cold-mixed epoxy asphalt, filling a gap in existing standards and accurately assessing its compatibility and stability.
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Figure CN116026801B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of road engineering materials, and particularly relates to a method for evaluating storage stability of cold-mixed epoxy asphalt. BACKGROUND
[0002] Epoxy asphalt is an important steel bridge deck paving material. According to different mixing temperatures, it can be generally divided into hot-mixed epoxy asphalt mixed at high temperature and cold-mixed epoxy asphalt mixed at normal temperature. In order to achieve the goal of normal temperature mixing, a large amount of organic solvent needs to be added to the cold-mixed epoxy asphalt to reduce the viscosity of the system, which often leads to segregation of the cold-mixed epoxy asphalt. At the same time, due to the differences in physical and chemical properties of epoxy resin and asphalt, the cold-mixed epoxy asphalt will also segregate if the preparation process is improper. Once the cold-mixed epoxy asphalt segregates, the use performance of the material will be seriously affected. However, the evaluation of the storage stability of the cold-mixed epoxy asphalt is basically in the blank stage at present. Therefore, it is necessary to quickly detect the storage stability of the cold-mixed epoxy asphalt. SUMMARY
[0003] The present application aims to overcome the deficiencies in the prior art and provide a method for evaluating storage stability of cold-mixed epoxy asphalt.
[0004] To achieve the above-mentioned purpose, the present application provides the following technical scheme:
[0005] A method for evaluating storage stability of cold-mixed epoxy asphalt comprises the following operation steps:
[0006] Step 1: preparation before sample storage and placement;
[0007] Step 2: method for sample storage and placement;
[0008] Step 3: qualitative evaluation method for sample storage stability;
[0009] Step 4: quantitative evaluation method for sample storage stability;
[0010] Step 5: grade division method for sample storage stability.
[0011] Step 1 comprises:
[0012] Step 11: uniformly stirring the prepared cold-mixed epoxy asphalt B component;
[0013] Step 12: placing the uniformly stirred cold-mixed epoxy asphalt B component into a segregation aluminum tube;
[0014] Step 13: weighing the cold-mixed epoxy asphalt A component for standby use.
[0015] The cold-mixed epoxy asphalt B component comprises the following components in parts by weight: 40-50 parts of base asphalt, 28-30 parts of acetone solvent, 50-55 parts of polyamide curing agent, 25-30 parts of epoxy soybean oil, 1-3 parts of KH550 silane coupling agent, and 1-3 parts of polydimethylsiloxane defoaming agent.
[0016] The cold-mixed epoxy asphalt A component is an epoxy resin.
[0017] Step 2 comprises:
[0018] Step 21: Place the isolated aluminum tube into a centrifuge and centrifuge at 600-1200 rpm for 10-20 min;
[0019] Step 22: Place the isolated aluminum tube after centrifugation at room temperature for at least 1 h;
[0020] Step 23: Take equal amounts of B component solution from the upper and lower ends of the isolated aluminum tube, add the same mass of A component as the sampled B component, stir uniformly, and place at room temperature for standby, to obtain an upper end cold-mixed epoxy asphalt mixed sample and a lower end cold-mixed epoxy asphalt mixed sample;
[0021] Step 24: Take a part of the upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample in the isolated aluminum tube, respectively, and place at room temperature for at least 24 h, and then place in a 50-60°C blast drying oven for at least 48 h, to obtain an upper end cold-mixed epoxy asphalt cured product and a lower end cold-mixed epoxy asphalt cured product for standby.
[0022] Step 3 comprises:
[0023] Step 31: Dip 4-6 μL of the mixture from the upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample, respectively, onto a glass slide, then cover with a cover glass, and stand for at least 30 min as a sample for fluorescence microscope observation;
[0024] Step 32: In the sample, the epoxy resin and polyamide curing agent emit fluorescence under high-pressure mercury lamp irradiation, and the asphalt cannot emit fluorescence and appears black. The phase distribution of the asphalt and the epoxy resin of the cold-mixed epoxy asphalt is observed by fluorescence microscope, and the compatibility and stability of the cold-mixed epoxy asphalt are qualitatively evaluated;
[0025] When the asphalt particle diameter distribution in the fluorescence microscope photograph is uniform, the asphalt is dispersed in the continuous phase of the epoxy resin as a dispersed phase, is distributed like small islands in the ocean, and is uniformly distributed, i.e., presents an "island-in-sea" structure, indicating that the storage stability of the cold-mixed epoxy asphalt is good; when the size uniformity of the asphalt phase particle size in the fluorescence microscope photograph is relatively poor, the storage stability is not good.
[0026] Step 4 comprises:
[0027] Step 41: Stirring the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in step 2 at 500-1000 rpm for at least 3 min respectively;
[0028] Step 42: Sampling the uniformly mixed upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture to prepare fluorescence microscope samples, and observing at least 30 pictures in the field of view of the fluorescence microscope randomly;
[0029] Step 43: Importing all the fluorescence microscope pictures of the collected upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture into Image Pro Plus 6.0 (IPP 6.0) software respectively;
[0030] Step 44: Image gray processing, using different gray scales to represent the resin phase and the asphalt phase;
[0031] Step 45: Gray scale reinforcement, enhancing the color difference between the asphalt phase and the resin phase;
[0032] Step 46: Re-scaling, calibrating the image, and the IPP 6.0 software identifying the asphalt and the resin in the image;
[0033] Step 47: Calculating the particle size, selecting the particle size of the asphalt phase as the calculation object, and obtaining an initial particle size data;
[0034] Step 48: Splitting the connected particles, re-analyzing and counting, splitting the selected connected particles in the image, and updating the initial particle size data to obtain the asphalt particle size distribution range μ;
[0035] Step 49: Calculating the densities of the upper end cold-mixed epoxy asphalt solidified substance and the lower end cold-mixed epoxy asphalt solidified substance in the segregation aluminum tube in step 2 respectively, and the density difference between the two is called the segregation rate ρ, which is used to assist in evaluating the compatibility and stability of the cold-mixed epoxy asphalt.
[0036] Step 5 comprises:
[0037] Step 51: Dividing the storage stability of the cold-mixed epoxy asphalt into different grades according to the segregation rate ρ, the asphalt particle size distribution range μ, and the asphalt quantity Q;
[0038] Step 52: Calculating the density of the upper end cold-mixed epoxy asphalt solidified substance in the segregation aluminum tube as ρ1, and the density of the lower end cold-mixed epoxy asphalt solidified substance in the segregation aluminum tube as ρ2, i.e. the segregation rate ρ = | ρ1- ρ2 |. When the segregation rate ρ ≤ 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as Class A; when the segregation rate ρ > 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as Class B;
[0039] Step 53: when the asphalt particle size distribution of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the aluminum tube is both μ≤25 μm, the cold-mixed epoxy asphalt frequency curve shows a "thin high" shape, and the storage stability of the cold-mixed epoxy asphalt is classified as A'; when the asphalt particle size distribution of the cold-mixed epoxy asphalt in the aluminum tube is one end μ≤25 μm and the other end μ>25 μm, or the asphalt particle size distribution of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the aluminum tube is both μ>25 μm, one end of the cold-mixed epoxy asphalt frequency curve shows a "thin high" shape, the other end shows a "wide short" shape, or both ends show a "wide short" shape, and the storage stability of the cold-mixed epoxy asphalt is classified as B';
[0040] Step 54: the asphalt quantity Q of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the aluminum tube is calculated by the particle size frequency distribution, when the asphalt quantity of the upper end and the lower end in the aluminum tube is both Q≥2500, the storage stability of the cold-mixed epoxy asphalt is classified as A"; when the asphalt quantity of one end is Q≥2500 and the other end is Q<2500, or the asphalt quantity of both ends is Q<2500, the storage stability of the cold-mixed epoxy asphalt is classified as B";
[0041] When the storage stability of the cold-mixed epoxy asphalt is classified as AA'A", the storage stability of the cold-mixed epoxy asphalt is optimal.
[0042] When the storage stability of the cold-mixed epoxy asphalt is classified as AA'B", AB'A" or BA'A", the storage stability of the cold-mixed epoxy asphalt is good.
[0043] When the storage stability of the cold-mixed epoxy asphalt is classified as AA'A", AA'B", AB'A" or BA'A" except, the storage stability of the cold-mixed epoxy asphalt is poor.
[0044] The epoxy resin is an E-51 type epoxy resin.
[0045] The type of the base asphalt includes B-SK70, B-GS70, B-SK90 or B-KL90.
[0046] Compared with the prior art, the present application has the following beneficial effects: the test scheme of the present application can evaluate the storage stability of the existing cold-mixed epoxy asphalt, and the method fills the blank of the existing cold-mixed epoxy asphalt related specification for storage stability evaluation.
[0047] The evaluation method of the present application can not only qualitatively evaluate the storage stability of the cold-mixed epoxy asphalt, but also quantitatively evaluate the storage stability of the cold-mixed epoxy asphalt, and the method fills the blank of the existing steel bridge deck pavement related specification for cold-mixed epoxy asphalt storage stability evaluation. BRIEF DESCRIPTION OF DRAWINGS
[0048] Figure 1 FM image of cold-mixed epoxy asphalt of the present application is shown;
[0049] Figure 2 FM image of cold-mixed epoxy asphalt of the present application after centrifugation is shown;
[0050] Figure 3 IPP 6.0 image processing step schematic diagram of cold-mixed epoxy asphalt of the present application is shown;
[0051] Figure 4 Graph showing the particle size distribution of the asphalt phase in the cold-mixed epoxy asphalt of the present application. DETAILED DESCRIPTION
[0052] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of the present application.
[0053] Example 1
[0054] An evaluation method for the storage stability of cold-mixed epoxy asphalt, the specific steps include:
[0055] (1) Select the base asphalt with penetration grade of 70 and 90 which are most used in the field of roads and bridges. Stir the B components of cold-mixed epoxy asphalt prepared from four different asphalts of SK70 (Korea), GS70 (Korea), SK90 (Korea) and KL90 (Karamay) uniformly, and then put them into segregation aluminum tubes;
[0056] (2) Put the segregation aluminum tubes into a centrifuge at 600 rpm for 20 min, and then immediately place the segregation aluminum tubes after centrifugation at room temperature for 1 h. The segregation aluminum tube is an aluminum tube for asphalt segregation test.
[0057] (3) Take equal amounts of solution from the upper and lower ends of the segregation aluminum tube, and add the A component according to the mass ratio of 1:1 after stirring uniformly, to obtain the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture, which are placed at room temperature for standby.
[0058] (4) Take 5 μL of sample from the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture solution with a paperclip, respectively, to prepare samples for fluorescence microscope observation, and observe the phase distribution of asphalt and epoxy resin of cold-mixed epoxy asphalt by fluorescence microscope.
[0059] In the cold-mixed epoxy asphalt, the epoxy resin and curing agent can emit fluorescence under the irradiation of high-pressure mercury lamp, but the asphalt cannot emit fluorescence and appears black. When the asphalt particle diameter in the fluorescence microscope photograph is uniformly distributed, the asphalt is dispersed in the continuous phase of the epoxy resin as the dispersed phase, like small islands dispersed in the ocean, and is uniformly distributed, that is, a "sea-island" structure is presented, as shown in Figure 1 (a) and (b) in FIG. 1, indicating that the storage stability of the cold-mixed epoxy asphalt is good; when the size uniformity of the asphalt phase particle diameter in the fluorescence microscope photograph is relatively poor, as shown in Figure 1 (c) and (d) in FIG. 1, the storage stability is not good.
[0060] As can be seen from Figure 2 , the upper part of the cold-mixed epoxy asphalt has uniformly distributed asphalt particles and presents a "sea-island" structure, indicating that the storage stability of the cold-mixed epoxy asphalt is good, while the lower part of the cold-mixed epoxy asphalt has unevenly distributed asphalt particles, indicating that the storage stability is slightly poor.
[0061] (5) As shown in Figure 3 , the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in step 3 are stirred at 500 rpm for 3 min, respectively, and fluorescence microscope samples are prepared by sampling, respectively, and observed. Randomly selected 30 pictures in the fluorescence microscope field of view are collected to import the fluorescence microscope photographs of the cold-mixed epoxy asphalt into Image Pro Plus 6.0 (IPP6.0) software, and the following operations are performed: ① image gray processing, the resin phase and the asphalt phase are represented by different gray scales; ② gray scale reinforcement, enhancing the color difference between the asphalt phase and the resin phase; ③ re-ruler, calibrating the image, and the software recognizes the image content; ④ calculating the particle diameter, selecting the calculation object, and obtaining an initial particle diameter data; ⑤ separating the connected particles, and re-counting and analyzing the connected particles selected in the image to update the statistical results.
[0062] (6) The upper and lower end, part of the cold-mixed epoxy asphalt mixture in the aluminum tube in step 3 is placed in a 60℃ air-drying oven for 48h after being placed at room temperature for 24h to obtain cold-mixed asphalt curing products, and the densities of the upper and lower end curing products of the cold-mixed epoxy asphalt are calculated to obtain the segregation rate.
[0063] Through calculation, the densities of the upper (lower) end of the epoxy resin solution prepared by the four kinds of asphalt B-SK70, B-GS70, B-SK90 and B-KL90 are 1.31g / cm 3 (1.23g / cm 3 ), 1.25g / cm 3 (1.20g / cm 3 ), 1.53g / cm 3 (1.18g / cm3 ), 1.55g / cm 3 (1.15g / cm 3 The segregation rates ρ were 0.08 g / cm³. 3 0.05g / cm 3 0.35g / cm 3 0.4g / cm 3 The particle size distribution ranges (μ) of the upper (lower) asphalt were 28μm (15μm), 20μm (23μm), 70μm (40μm), and 75μm (25μm), respectively; the number of asphalt particles at the upper (lower) ends were 2530 (2620), 2620 (4750), 300 (1550), and 250 (2350), respectively. Therefore, the storage stability classifications of cold-mix epoxy asphalt prepared from these four asphalts are AB'A", AA'A", BB'B", and BB'B", respectively. That is, the cold-mix epoxy asphalt prepared with B-GS70 has the best storage stability; the cold-mix epoxy asphalt prepared with B-SK70 has good storage stability; and the cold-mix epoxy asphalt prepared with B-SK90 and B-KL90 has poor storage stability. Figure 4 As shown, the frequency response curve of B-GS70 exhibits a "tall and slender" shape, with the particle size distribution mainly concentrated around 20–30 μm. In contrast, the other three types of epoxy asphalt prepared from asphalt show a wider and shorter peak distribution in their particle size curves, with larger particle sizes mainly concentrated around 25–75 μm. This indicates that the asphalt in the cold-mix epoxy asphalt prepared using GS70 base asphalt has a better dispersion effect in the epoxy resin. Furthermore, the figure also shows that the particle size distribution of epoxy asphalt prepared from No. 70 asphalt is more concentrated than that of epoxy asphalt prepared from No. 90 asphalt. This suggests that the cold-mix epoxy asphalt prepared from No. 70 asphalt has better compatibility with the resin, and that the type of asphalt has a significant impact on the compatibility and storage stability of cold-mix epoxy asphalt.
[0064] Example 2
[0065] A method for evaluating the storage stability of cold-mixed epoxy asphalt includes the following steps:
[0066] Step 1: Preparations before sample storage and placement;
[0067] Step 11: Stir the prepared cold-mix epoxy asphalt component B evenly;
[0068] Step 12: Place the well-stirred cold-mixed epoxy asphalt component B into the segregated aluminum tube;
[0069] Step 13: Weigh the cold-mixed epoxy asphalt component A for later use.
[0070] The cold-mixed epoxy asphalt B component comprises the following components in parts by weight: 40-50 parts of base asphalt, 28-30 parts of acetone solvent, 50-55 parts of polyamide curing agent, 25-30 parts of epoxy soybean oil, 1-3 parts of KH550 silane coupling agent, and 1-3 parts of polydimethylsiloxane defoaming agent.
[0071] The cold-mixed epoxy asphalt A component is an epoxy resin.
[0072] Step 2: sample storage placement method;
[0073] Step 21: place the isolated aluminum tube into a centrifuge for centrifugation at 1200 rpm for 10 min;
[0074] Step 22: place the isolated aluminum tube after centrifugation at room temperature for 2 h;
[0075] Step 23: take equal amounts of B component solution from the upper and lower ends of the isolated aluminum tube, add the same mass of A component as the sampled B component, stir uniformly, and place at room temperature for standby, to obtain upper and lower cold-mixed epoxy asphalt mixture samples;
[0076] Step 24: take part of the upper and lower cold-mixed epoxy asphalt mixture samples from the isolated aluminum tube, respectively, and place at room temperature for 30 h, and then place in a 50°C blast drying oven for 60 h, to obtain upper and lower cold-mixed epoxy asphalt cured products, for standby.
[0077] Step 3: sample storage stability qualitative evaluation method;
[0078] Step 31: dip 4 μL of the mixture from the upper and lower cold-mixed epoxy asphalt mixture samples, respectively, onto a glass slide, then cover with a cover glass, and stand for 30 min as a sample for fluorescence microscope observation;
[0079] Step 32: in the sample, the epoxy resin and polyamide curing agent emit fluorescence under high-pressure mercury lamp irradiation, and the asphalt cannot emit fluorescence and appears black, the phase distribution of the asphalt and epoxy resin of the cold-mixed epoxy asphalt is observed by fluorescence microscope, and the compatibility stability of the cold-mixed epoxy asphalt is qualitatively evaluated;
[0080] When the asphalt particle diameter distribution in the fluorescence microscope photograph is uniform, the asphalt is dispersed in the continuous phase of the epoxy resin as a dispersed phase, like islands dispersed in the ocean, and the distribution is uniform, i.e. presents an “island-in-sea” structure, indicating that the storage stability of the cold-mixed epoxy asphalt is good; when the uniformity of the size of the asphalt phase particle diameter in the fluorescence microscope photograph is relatively poor, the storage stability is not good.
[0081] Step 4: sample storage stability quantitative evaluation method;
[0082] Step 41: Stir the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in step 2 at 1000 rpm for 5 min respectively;
[0083] Step 42: Sample 4-6 μL of the uniformly mixed upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture respectively, which can be 4 μL, 5 μL or 6 μL, to prepare a fluorescence microscope sample and observe, and randomly select 40 pictures in the field of view of the fluorescence microscope;
[0084] Step 43: Import the 40 fluorescence microscope pictures of the collected upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture respectively into IPP 6.0 software;
[0085] Step 44: Image gray processing, the resin phase and the asphalt phase are represented by different gray scales;
[0086] Step 45: Gray scale reinforcement, enhance the color difference between the asphalt phase and the resin phase;
[0087] Step 46: Re-scale, calibrate the image, and the IPP 6.0 software recognizes the asphalt and resin in the image;
[0088] Step 47: Calculate the particle size, select the particle size of the asphalt phase as the calculation object, and obtain an initial particle size data;
[0089] Step 48: Separate the connected particles, and re-analyze and analyze the selected connected particles in the image, update the initial particle size data to obtain the asphalt particle size distribution range μ;
[0090] Step 49: Calculate the densities of the upper end cold-mixed epoxy asphalt solidified material and the lower end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube in step 2 respectively, and the density difference between the two is called the segregation rate ρ, which is used to assist in evaluating the compatibility and stability of the cold-mixed epoxy asphalt.
[0091] Step 5: Grade division method of sample storage stability;
[0092] Step 51: According to the segregation rate ρ, the asphalt particle size distribution range μ and the asphalt quantity Q, the storage stability of the cold-mixed epoxy asphalt is graded;
[0093] Step 52: Calculate the density of the upper end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube as ρ1, and the density of the lower end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube as ρ2, that is, the segregation rate ρ = | ρ1- ρ2 |. When the segregation rate ρ ≤ 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as A; when the segregation rate ρ > 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as B;
[0094] Step 53: When the asphalt particle size distribution of the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in the aluminum tube is μ≤25 μm, the cold-mixed epoxy asphalt frequency curve shows a "thin high" shape, and the storage stability of the cold-mixed epoxy asphalt is classified as A' class; when the asphalt particle size distribution of the cold-mixed epoxy asphalt in the aluminum tube is μ≤25 μm at one end, μ>25 μm at the other end, and the asphalt particle size distribution of the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in the aluminum tube is μ>25 μm, one end of the cold-mixed epoxy asphalt frequency curve shows a "thin high" shape, the other end shows a "wide short" shape, or both ends show a "wide short" shape, at this time, the storage stability of the cold-mixed epoxy asphalt is classified as B' class;
[0095] Step 54: The asphalt quantity Q of the upper end cold-mixed epoxy asphalt mixture and the lower end cold-mixed epoxy asphalt mixture in the aluminum tube is calculated by particle size frequency distribution (calculated directly by using Image-Pro plus 6.0 (IPP) analysis statistical software), and the asphalt quantity Q is the number of asphalts in the picture in each field of view of the fluorescence microscope,
[0096] When the asphalt quantity of the upper end and the lower end in the aluminum tube is Q≥2500, the storage stability of the cold-mixed epoxy asphalt is classified as A" class; when the asphalt quantity of one end in the aluminum tube is Q≥2500, and the asphalt quantity of the other end is Q<2500; or the asphalt quantity of both ends is Q<2500, the storage stability of the cold-mixed epoxy asphalt is classified as B" class.
[0097] When the storage stability of the cold-mixed epoxy asphalt is classified as AA' A", the storage stability of the cold-mixed epoxy asphalt is optimal.
[0098] When the storage stability of the cold-mixed epoxy asphalt is classified as AA'B", AB'A", or BA'A", the storage stability of the cold-mixed epoxy asphalt is good.
[0099] When the storage stability of the cold-mixed epoxy asphalt is classified as AA' A", AA'B", AB'A", or BA'A" except, the storage stability of the cold-mixed epoxy asphalt is poor.
[0100] Example 3
[0101] The difference between this example and Example 1 is that 6 μL of sample is taken in step 31.
[0102] It will be obvious to a person skilled in the art that the application is not limited to the details of the foregoing exemplary embodiments and can be implemented in other concrete forms without departing from the spirit or essential characteristics of the application. The embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. No reference signs in the claims should be considered as limiting the scope of the claims to the identity of the reference signs therein.
[0103] Furthermore, it should be understood that although the description is made on the basis of the embodiments, not every embodiment contains only one independent technical solution, and the description of the specification is only for the sake of clarity, and those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that those skilled in the art can understand.
Claims
1. A method for evaluating storage stability of cold-mixed epoxy asphalt, characterized by: The method comprises the following steps: Step 1: sample storage preparation before placement; Step 2: sample storage placement method; Step 3: qualitative evaluation method of sample storage stability; Step 4: quantitative evaluation method of sample storage stability; Step 5: sample storage stability grade division method; Step 1 comprises: Step 11: stirring the prepared cold-mixed epoxy asphalt B component uniformly; Step 12: placing the uniformly stirred cold-mixed epoxy asphalt B component into a separation aluminum tube; Step 13: weighing the cold-mixed epoxy asphalt A component for standby; The cold-mixed epoxy asphalt B component comprises the following components in parts by weight: 40-50 parts of base asphalt, 28-30 parts of acetone solvent, 50-55 parts of polyamide curing agent, 25-30 parts of epoxy soybean oil, 1-3 parts of KH550 silane coupling agent, and 1-3 parts of polydimethylsiloxane defoaming agent; The cold-mixed epoxy asphalt A component is an epoxy resin; Step 2 comprises: Step 21: placing the separation aluminum tube into a centrifuge to centrifuge at 600-1200 rpm for 10-20 min; Step 22: placing the separation aluminum tube after centrifugation at room temperature for at least 1 h; Step 23: taking equal amounts of B component solution from the upper and lower ends of the separation aluminum tube, adding A component with the same mass as the sampled B component, stirring uniformly, and placing at room temperature for standby to obtain an upper end cold-mixed epoxy asphalt mixed sample and a lower end cold-mixed epoxy asphalt mixed sample; Step 24: taking part of the upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample in the separation aluminum tube, placing at room temperature for at least 24 h, and then placing in a 50-60℃ air-drying oven for at least 48 h to obtain upper end cold-mixed epoxy asphalt solidified product and lower end cold-mixed epoxy asphalt solidified product for standby; Step 3 comprises: Step 31: dipping 4-6µL of the mixture from the upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample respectively onto a glass slide, then covering with a cover glass, and standing for at least 30 min as a sample for fluorescence microscope observation; Step 32: in the sample, the epoxy resin and polyamide curing agent emit fluorescence under high-pressure mercury lamp irradiation, and the asphalt cannot emit fluorescence and appears black, and the phase distribution of the asphalt and the epoxy resin of the cold-mixed epoxy asphalt is observed by fluorescence microscope to qualitatively evaluate the compatibility stability of the cold-mixed epoxy asphalt; When the asphalt particle diameter distribution in the fluorescence microscope photo is uniform, the asphalt is dispersed in the continuous phase of the epoxy resin as a dispersed phase, is distributed like small islands in the ocean, and is uniformly distributed, that is, presents an "island-in-sea" structure, indicating that the storage stability of the cold-mixed epoxy asphalt is good; Step 4 comprises: Step 41: stirring the upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample in step 2 at 500-1000 rpm for at least 3 min; Step 42: sampling the uniformly mixed upper end cold-mixed epoxy asphalt mixed sample and the lower end cold-mixed epoxy asphalt mixed sample to prepare fluorescence microscope samples, and observing, and randomly selecting at least 30 pictures in the fluorescence microscope field of view; Step 43: Import all the fluorescence microscope photos of the collected upper end cold-mixed epoxy asphalt mixture sample and lower end cold-mixed epoxy asphalt mixture sample into IPP 6.0 software respectively; Step 44: Image gray processing, the resin phase and the asphalt phase are represented by different gray scales; Step 45: Gray scale reinforcement, enhance the color difference between the asphalt phase and the resin phase; Step 46: Re-scale, calibrate the image, and IPP 6.0 software identifies the asphalt and resin in the image; Step 47: Calculate the particle size, select the particle size of the asphalt phase for calculation, and obtain an initial particle size data; Step 48: Separate the connected particles, and perform statistical analysis again to separate the selected connected particles in the image, update the initial particle size data to obtain the asphalt particle size distribution range µ; Step 49: Calculate the densities of the upper end cold-mixed epoxy asphalt solidified material and the lower end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube in step 2 respectively, and the density difference between the two is called the segregation rate ρ, which is used to assist in evaluating the compatibility and stability of the cold-mixed epoxy asphalt; Step 5 includes: Step 51: The storage stability of cold-mixed epoxy asphalt is graded according to the dissociation rate ρ , the asphalt particle size distribution range µ, and the asphalt quantity Q. Step 52: Calculate the density of the upper end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube as ρ1, and the density of the lower end cold-mixed epoxy asphalt solidified material in the segregation aluminum tube as ρ2, that is, the segregation rate ρ = | ρ1- ρ2 |; when the segregation rate ρ ≤ 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as A; when the segregation rate ρ > 0.2, the storage stability of the cold-mixed epoxy asphalt is classified as B; Step 53: When the asphalt particle size distribution concentration range of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the segregation aluminum tube is all µ ≤ 25 μm, the cold-mixed epoxy asphalt frequency curve shows a "tall and thin" shape, and the storage stability of the cold-mixed epoxy asphalt is classified as A'; when the asphalt particle size distribution concentration range of the cold-mixed epoxy asphalt in the segregation aluminum tube is one end µ ≤ 25 μm, one end µ > 25 μm, and the asphalt particle size distribution concentration range of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the segregation aluminum tube is all µ > 25 μm, one end of the cold-mixed epoxy asphalt frequency curve shows a "tall and thin" shape, the other end shows a "wide and short" shape, or both ends show a "wide and short" shape, and the storage stability of the cold-mixed epoxy asphalt is classified as B'; Step 54: Calculate the asphalt quantity Q of the upper end cold-mixed epoxy asphalt mixture sample and the lower end cold-mixed epoxy asphalt mixture sample in the segregation aluminum tube through the particle size frequency distribution; when the asphalt quantity Q of both the upper end and the lower end in the segregation aluminum tube is all Q ≥ 2500, the storage stability of the cold-mixed epoxy asphalt is classified as A''; when the asphalt quantity Q of one end is Q ≥ 2500 and the asphalt quantity Q of the other end is Q < 2500, or the asphalt quantity Q of both ends is Q < 2500, the storage stability of the cold-mixed epoxy asphalt is classified as B''; When the storage stability of the cold-mixed epoxy asphalt is classified as AA' A'', the storage stability of the cold-mixed epoxy asphalt is optimal; When the storage stability of the cold-mixed epoxy asphalt is classified as AA' B'', AB' A'', BA' A'', the storage stability of the cold-mixed epoxy asphalt is good; The storage stability of the cold-mixed epoxy asphalt is poor except when the storage stability of the cold-mixed epoxy asphalt is classified as AA'A'', AA'B'', AB'A'', or BA'A''.
2. The evaluation method according to claim 1, characterized by: The epoxy resin is an E-51 type epoxy resin.
3. The evaluation method according to claim 1, characterized by: The type of the base asphalt includes B-SK70, B-GS70, B-SK90, or B-KL90.
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