CN115353748B - Waste fan blade composite fiber and preparation method of waste fan blade composite fiber and SBS composite modified asphalt - Google Patents

Waste fan blade composite fiber and preparation method of waste fan blade composite fiber and SBS composite modified asphalt Download PDF

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CN115353748B
CN115353748B CN202211173568.4A CN202211173568A CN115353748B CN 115353748 B CN115353748 B CN 115353748B CN 202211173568 A CN202211173568 A CN 202211173568A CN 115353748 B CN115353748 B CN 115353748B
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wfb
asphalt
modified asphalt
sbs
silane coupling
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CN115353748A (en
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聂忆华
刘庆
彭红卫
高闻靖
龙雷翔
毛惺
钟世雄
黄新摇
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Hunan University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L2207/20Recycled plastic

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Abstract

The invention discloses a waste fan blade composite fiber and a preparation method of the waste fan blade composite fiber and SBS composite modified asphalt, crushing and screening waste fan blades, and selecting waste fan blade composite fiber with the particle size of 0.15-0.3mm, namely WFB; heating the matrix asphalt to a molten state, adding the selected WFB, and swelling a mixture of the WFB and the matrix asphalt; and (3) shearing the mixture of the WFB and the matrix asphalt after swelling at a high speed at 140-160 ℃, and then keeping the temperature at 145+/-1 ℃ for 10min to obtain the WFB modified asphalt. Heating matrix asphalt to a molten state, mixing SBS, preparing SBS modified asphalt, adding selected WFB, uniformly stirring, swelling for 10min at 160+/-1 ℃, adjusting the temperature of the blend to 140-160 ℃ and shearing at high speed, and developing for 10min at a constant temperature of 150+/-1 ℃ to obtain SBS/WFB compound modified asphalt, thereby filling the blank.

Description

Waste fan blade composite fiber and preparation method of waste fan blade composite fiber and SBS composite modified asphalt
Technical Field
The invention belongs to the field of modified asphalt preparation, and relates to a waste fan blade composite fiber (WFB for short) and a preparation method of SBS complex doped modified asphalt.
Background
Wind power generation is one of sustainable green development industry, but waste fan blades are large in size and not easy to degrade, no mature, economical and environment-friendly waste fan blade recovery treatment technology exists in the world at present, and most of treatment modes are concentrated storage and small incineration power generation treatment at present. The fan blades are mainly stacked and buried as solid waste, so that a large amount of land resources are wasted, and toxic substances such as styrene and the like are separated out to pollute soil environment and groundwater and influence life health. In order to realize the environment protection and the green development of resources, the development and reuse research of the recycled materials of the waste fan blades is needed.
The common recovery treatment method for the waste fan blade mainly comprises physical recovery, chemical recovery, energy recovery and the like. The physical recovery method is characterized in that the waste fan blade is reused as a modifier, a filler and the like after being removed, cut, cleaned and crushed, the treatment cost is low, the flow is simple, and the method is the most common method for treating the waste fan blade at present. The chemical recovery method is various, the pyrolysis method is to decompose the waste fan blade material under the anoxic condition, the resin is organic solid waste, and pure glass fiber/carbon fiber can be recovered by heating and cracking the resin, but pyrolysis equipment is expensive and has higher cost; the supercritical fluid method is used as a novel technology, is clean and pollution-free, but has the advantages of severe critical conditions, low safety coefficient and test stage at present; the dissolution method is mild in treatment, but the organic solvent is large in use amount and long in reaction time. The energy recovery method is to convert the heat energy generated by the incineration of the wastes containing the organic matters into other energy, and the treatment is simple, but toxic and harmful gas can be released in the incineration process, and secondary pollution can be caused to the environment due to improper ash treatment after the incineration. At present, after mechanically crushing, retired waste fan blades are used as a filler to be doped into cement products to realize recycling, or the retired waste fan blades are used for replacing components such as gravel, clay and the like in cement to realize recycling of the waste fan blades.
Asphalt pavement is widely applied to roads of various grades in China by virtue of excellent road performance. In order to improve the performance of the asphalt pavement, a great number of experimental researches are carried out on students at home and abroad, and various performances of an asphalt mixture prepared by adding various fibers into a common asphalt mixture are greatly improved. Research shows that the application research of various fibers in asphalt or asphalt mixture is rich, the carbon fiber reinforced asphalt can improve the mechanical property, the carbon fiber reinforced composite material (CFRP) has better durability, and the glass fiber can be used as a reinforcing material in the asphalt mixture to provide additional tensile strength.
Most of the waste fan blades are made of high polymer fiber materials and mainly comprise GFRP (glass fiber reinforced composite) and CFRP (carbon fiber reinforced composite). At present, the research of waste fan blades in road modified asphalt belongs to the blank, so that the research on the preparation process and technical performance of WFB modified asphalt provides a new thought for recycling solid waste fan blades, and provides a novel modified asphalt material for better improving the road performance of asphalt pavement in China, and has important significance.
Disclosure of Invention
The embodiment of the invention aims to provide a waste fan blade composite fiber and a preparation method of the waste fan blade composite fiber and SBS (styrene-butadiene-styrene) composite modified asphalt, so as to solve the problems that the conventional waste fan blade composite fiber is difficult to recycle with high value and the road fiber modified asphalt is high in price, and the WFB is blank in the road modified asphalt.
The technical scheme adopted by the embodiment of the invention is as follows: the preparation method of the waste fan blade composite fiber modified asphalt comprises the following steps:
crushing and screening waste fan blades, and selecting waste fan blade crushed materials with the particle size of 0.15-0.3mm as waste fan blade composite fibers, namely WFB;
heating matrix asphalt to a molten state, and mixing the selected WFB to the matrix asphalt in the molten state, wherein the addition amount of the WFB is 0.5-6% of the mass of the matrix asphalt;
swelling the WFB and matrix asphalt mixture;
shearing the mixture of the WFB and the matrix asphalt after swelling at a high speed at a temperature of 140-160 ℃;
and (3) keeping the temperature of the sheared blend of the WFB and the matrix asphalt at 145+/-1 ℃ for 10min to obtain the WFB modified asphalt.
Further, when the selected WFB is mixed into the matrix asphalt in a molten state, the dry WFB is added into the matrix asphalt for 3 times under the conditions of heating and stirring, so that uniform dispersion and stable temperature are ensured.
Further, heating the base asphalt to a molten state at 145+ -5deg.C;
developing for 30-40 min at the constant temperature of 160+/-1 ℃, and stirring the WFB and matrix asphalt mixture for thermal insulation swelling;
the shearing rate of high-speed shearing is 4000-6000 rad/min, and the shearing time is 20-60 min.
Further, the addition amount of WFB is 2% of the mass of the matrix asphalt; the constant temperature development time is 30min; the high-speed shearing temperature is 140 ℃, the shearing rate is 4000r/min, and the shearing time is 40min.
Further, the surface treatment of WFB is carried out by adopting a silane coupling agent, and then the modified asphalt is prepared by adopting the WFB after the surface treatment.
Further, WFB was surface treated with a silane coupling agent solution by the following method:
heating WFB in an oven at 230+ -1deg.C for 1h, cooling, soaking in acetone solution for 1h, taking out, cleaning and air drying; then soaking in a silane coupling agent solution for 1h, drying in an oven at 120+/-1 ℃, taking out and cooling for standby;
the mixing amount of the silane coupling agent is 30% of the mass of the selected WFB;
the mass ratio of silane, ethanol and water in the silane coupling agent solution is 5:85:10.
Further, WFB was surface treated with A-188 silane coupling agent.
The embodiment of the invention adopts another technical scheme that: the preparation method of the waste fan blade composite fiber and SBS compound modified asphalt comprises the following steps:
crushing and screening waste fan blades, and selecting waste fan blade composite fibers with the particle size of 0.15-0.3mm, namely WFB for later use;
heating matrix asphalt to a molten state, then doping SBS, heating to 160-170 ℃ and stirring at a high speed to prepare SBS modified asphalt, wherein the doping amount of SBS is 1-4% of the mass of the matrix asphalt;
adding the selected WFB, uniformly stirring, placing in an oven, and swelling for 10min at 160+/-1 ℃, wherein the doping amount of the WFB is 0.5% -4% of the mass of the SBS modified asphalt;
regulating the temperature of the blend of SBS modified asphalt and WFB to 140-160 ℃ and shearing at a high speed;
and developing the sheared blend of the SBS modified asphalt and the WFB for 10min at the constant temperature of 150+/-1 ℃ to obtain the SBS/WFB composite modified asphalt, namely the waste fan blade composite fiber and the SBS composite modified asphalt.
Further, heating the base asphalt to a molten state at 145+ -5deg.C;
the stirring speed of high-speed stirring is 2000+/-20 rad/min, and the stirring time is 20min;
the shearing rate of high-speed shearing is 4000-6000 rad/min, and the shearing time is 20-60 min.
Further, after swelling, adjusting the temperature of the blend of SBS modified asphalt and WFB to 140 ℃, and shearing for 40min under 4000 rad/min;
the optimal blending amount of SBS is 4% of the mass of matrix asphalt, and the optimal blending amount of WFB is 2% of the mass of SBS modified asphalt.
The embodiment of the invention has the beneficial effects that:
(1) Compared with the fiber adopted by the prior modified asphalt, the WFB has certain advantages in the aspects of wear resistance, production cost and modified asphalt pavement cost, solves the problems of difficult reutilization of high value of the WFB and high price of the fiber modified asphalt for roads, and fills the application gap of the WFB in the road modified asphalt;
(2) The research range of the road modified asphalt is enlarged, the WFB modified asphalt has low cost and good high-temperature performance, and a new choice is provided for the engineering application of the modified asphalt;
(3) The embodiment of the invention shows that the WFB modified asphalt has a certain feasibility and development prospect; the road modified asphalt is wide in application and large in WFB digestion, and is beneficial to social carbon reduction and emission reduction and green development;
(4) The preparation process of the WFB modified asphalt, which has guiding significance for production and application, is provided, and the modification mechanism of the WFB modified asphalt is revealed;
(5) The blending and performance rules of SBS/WFB complex blending modified asphalt are systematically researched, and the proportion of complex blending modified asphalt with excellent performance under each performance is given.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the best preparation of WFB modified asphalt.
Fig. 2 is a SEM image of three particle sizes of WFB.
FIG. 3 is a graph of WFB modified asphalt (three particle sizes) performance index at different loadings.
FIG. 4 is a graph of the results of tests on WFB modified asphalt (particle size C) at various loadings.
FIG. 5 is a factor bit level impact trend graph.
FIG. 6 is a diagram showing the mechanism of action of a silane coupling agent.
Fig. 7 is an SEM image of WFB at different magnification.
Fig. 8 is an SEM image of silane coupling agent treated WFB.
Fig. 9 is an XRD pattern of WFB before and after the silane coupling agent treatment.
FIG. 10 is a graph of WFB modified asphalt performance indicators after various silane coupling agent treatments.
FIG. 11 is a graph of WFB modified asphalt performance index after treatment with different types of silane coupling agents.
FIG. 12 is a graph of WFB modified asphalt performance index after treatment with varying amounts of silane coupling agent.
FIG. 13 is an infrared spectrum of WFB before and after treatment with a silane coupling agent.
FIG. 14 is an infrared spectrum of WFB modified asphalt before and after treatment with a silane coupling agent.
FIG. 15 is a flow chart of the preparation of SBS/WFB complex blended modified asphalt.
FIG. 16 is a graph of SBS/WFB complex blend modified asphalt temperature sensitivity index.
FIG. 17 is a graph of high temperature performance indicators for SBS/WFB complex blended modified asphalt.
FIG. 18 is a graph of SBS/WFB low temperature performance indicators for a remixed modified asphalt.
FIG. 19 is a graph of SBS/WFB complex blend modified asphalt plasticity temperature interval indicators.
FIG. 20 is a graph of the results of segregation test of a preferred four-group SBS/WFB complex blend modified asphalt.
FIG. 21 is a graph of the results of AFM three roughness and surface area differences for SBS/WFB complex blended modified asphalt.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of WFB modified asphalt, which comprises the following steps:
crushing and screening waste fan blades, and selecting waste fan blade composite fibers with the particle size of 0.15-0.3mm, namely WFB;
heating the base asphalt to a molten state at 145+ -5deg.C;
adding the selected WFB into the matrix asphalt in a molten state, and mixing, wherein the WFB is added for 3 times under the conditions of heating and stirring during mixing, so that the WFB and the matrix asphalt are fully fused, and the addition amount of the WFB is 0.5-6% of the mass of the matrix asphalt;
developing for 30-40 min at the constant temperature of 160+/-1 ℃ to swell the mixture of WFB and matrix asphalt;
shearing the mixture of the WFB and the matrix asphalt after swelling at a high speed for 20-60 min under the conditions of 140-160 ℃ and 4000-6000 rad/min;
and (3) keeping the temperature of the sheared blend of the WFB and the matrix asphalt at 145+/-1 ℃ for 10min to obtain the WFB modified asphalt.
In some embodiments, as shown in FIG. 1, the matrix pitch is heated to a molten state at 145℃and the selected WFB is added to the matrix pitch in the molten state under 145℃heating conditions;
developing for 30min at 160 ℃ with constant temperature, swelling the mixture of WFB and matrix asphalt, and properly heating and stirring to ensure asphalt fluidity;
shearing the mixture of the swollen WFB and the matrix asphalt at a high speed for 40min under the conditions of 140 ℃ and 4000 rad/min;
and (3) keeping the temperature of the sheared mixture of the WFB and the matrix asphalt at 145 ℃ for 10min to obtain the WFB modified asphalt.
The initial raw materials obtained by the WFB through mechanical crushing are screened, a shaking screening machine is used for screening, shaking screening time is set for 30min for ensuring the purity and consistency of the materials, and screening results are shown in Table 1.
TABLE 1 hierarchical screening of WFB raw materials
After sieving, the WFB crushed material is divided into a particle size A (less than 0.075 mm), a particle size B (0.075-0.15 mm), a particle size C (0.15-0.3 mm) and other materials with a sieve diameter greater than 0.3mm, and the performance test analysis for asphalt modification is mainly carried out aiming at A, B, C particle size researches, and results show that the asphalt adsorption capacity, heat resistance and moisture resistance of the WFB meet the use requirements for preparing modified asphalt and asphalt mixture.
To determine the selection of WFB, a Scanning Electron Microscope (SEM) test was performed on particle size A, B, C, the results of which are shown in FIG. 2. As can be seen from fig. 2, the particles having a particle size a were large, and it was determined that the particles were resin, the fiber diameter was about 15.1 μm, and the particles were short fibers, which was not conducive to the formation of a skeleton in the asphalt cement; the particle size of the particle size B is obviously increased, and the fiber is longer, but in practice, the physical method is difficult to separate the fiber from the resin; the fiber in the particle size C is more, the length is more than 200 mu m, the particle size is coarse, and the sieving is convenient. According to SEM microscopic test analysis, the particle size C (0.15-0.3 mm) is more suitable for modified asphalt.
Three index tests were performed on the particle size A, B, C and the WFB modified asphalt of different amounts, respectively, and the results are shown in FIG. 3. As can be seen from FIG. 3, the softening point value of the particle size C is higher in various blending amounts, the blending amount of the particle size C reaches 59.4 ℃ when being 2% of the mass of the matrix asphalt, and the temperature is improved by about 10 ℃ compared with the matrix asphalt, so that the high-temperature stability of the modified asphalt is improved, the softening point of the particle size C is increased greatly, the penetration value is larger, and the particle size C is suitable for the modified asphalt.
The blending amount of the modified asphalt with the particle size C was further studied, and the test results are shown in FIG. 4. As can be seen from fig. 4, the modified asphalt softening point increases significantly with the increase of the blending amount of the particle size C, and then remains stable, and the blending amount is 2% as an inflection point, so that the WFB modified asphalt has better high-temperature rutting resistance. The ductility and penetration of the modified asphalt decrease with the increase of the WFB doping amount, the doping amount is 4% and 6%, the ductility and penetration value is lower than the doping amount of 2%, the low-temperature performance is poor, and the optimum doping amount is determined to be 2%.
The inventor researches that constant temperature development time, shearing temperature, shearing rate and shearing time are key preparation process parameters influencing the performance of the modified asphalt, and designs L 9 (3 4 ) Four-factor three-level orthogonal test scheme is shown in table 2, and three technical indexes of the WFB modified asphalt prepared by the test scheme of table 2 are tested, and the results are shown in table 3.
Table 2 orthogonal test design scheme for WFB modified asphalt
TABLE 3 results of orthogonal test of WFB modified asphalt
As can be seen from Table 3, the 15℃ductility and 25℃penetration data were significantly changed with less fluctuation of softening point values in the 9 test protocols. Contrast matrix asphalt: the penetration degree is reduced, which shows that WFB can obviously increase the consistency of asphalt, so that the deformation resistance of matrix asphalt is improved; the ductility values are reduced to different degrees, which indicates that WFB reduces the ductility of the matrix asphalt; the softening point rises by about 5-17 ℃, which indicates that the WFB can improve the high-temperature performance of the matrix asphalt and is beneficial to improving the use stability of asphalt in high-temperature areas in summer. In order to determine the dominant and subordinate of the influence of different factor levels on asphalt indexes, visual analysis is carried out on test results, and a trend chart of influence factors is drawn, which is shown in tables 4 and 5.
TABLE 4 visual analysis of orthogonal test results
The significance ordering and the preferred scheme of the three index factors of the modified asphalt are shown in the table 4. As can be seen from Table 4 and FIG. 5, the influence of the factor B (preparation temperature) and the factor D (shear rate) on three indexes of penetration, ductility and softening point of the modified asphalt is most remarkable. The method aims at the good performance requirement of the modified asphalt, namely a higher softening point, a larger ductility and penetration value, analyzes the influence trend of the factor level on three indexes, further seeks the optimal preparation process of the modified asphalt under the controllable condition, provides an optimization scheme of the factor level of the WFB modified asphalt, and obtains the index of the modified asphalt by test, wherein the optimization scheme is shown in Table 5.
Table 5 optimization scheme for WFB modified asphalt preparation
Test label A development time/min B preparation temperature/. Degree.C C shear rate/r.min -1 D shear time/min
T 1 -A 1 B 1 C 1 D 1 30 140 4000 20
T 2 -A 1 B 1 C 1 D 2 30 140 4000 40
T 3 -A 1 B 2 C 1 D 1 30 160 4000 20
T 4 -A 1 B 2 C 1 D 2 30 160 4000 40
Table 6 Performance index of WFB modified asphalt optimization scheme
As can be seen from Table 6, the penetration of the four groups of tests is lower than that of the matrix asphalt (63/0.1 mm), and the shear deformation resistance of the modified asphalt is improved; the rotational viscosity value of the four groups of tests at 135 ℃ is at least 2.4 times higher than that of matrix asphalt (571 mPa.s), which shows that the high-temperature deformation resistance of the modified asphalt is greatly improved, and the construction requirement that the construction specification of highway asphalt pavement is not more than 3 Pa.s is satisfied; the softening points of the four groups of tests are improved compared with that of matrix asphalt (47 ℃), and the amplitudes are respectively as follows: 19%, 23%, 22% and 24% indicate that WFB can well improve the high-temperature stability of matrix asphalt; the test ductility is reduced, which indicates that the low-temperature anti-cracking performance index of the modified asphalt is reduced when the WFB is doped; the difference value of softening points of the WFB modified asphalt segregation test meets the requirement that the specification requirement is less than or equal to 2.5 ℃, which shows that the WFB modified asphalt has better storage stability; among four groups of WFB modified asphalt test indexes, the T2 has the advantages of minimum equivalent brittle point and temperature sensitivity coefficient, maximum equivalent softening point, and larger softening point and penetration, which indicates that the modified asphalt under the process has low temperature sensitivity, stable performance and better low-temperature performance.
The preparation process parameters are optimized through gray correlation analysis, and the correlation coefficients and the correlation degree of each index are shown in Table 7. As can be seen from table 7, the correlation of T2 is maximally the optimal preparation process parameter, which is consistent with the analysis results of the orthogonal test. The optimal preparation process parameters of the WFB modified asphalt are as follows: the constant temperature development time is 30min, the shearing temperature is 140 ℃, the shearing rate is 4000r/min, and the shearing time is 40min, as shown in figure 1.
TABLE 7 correlation coefficient and correlation degree of WFB modified asphalt optimization scheme
To investigate the impact of WFB functional group characteristics on modified asphalt performance, FTIR experiments were performed on WFB, matrix asphalt, WFB modified asphalt, see FIG. 14. As can be seen from fig. 14, the WFB modified asphalt is similar to the infrared spectrogram of the matrix asphalt, the positions of the absorption peaks in the functional group region and the fingerprint region are basically consistent, but the difference exists between the intensity of the absorption peaks, which indicates that no new functional group is generated after the matrix asphalt is doped with the waste fan blade material, the chemical structure of the asphalt is not affected, and only simple physical winding occurs. The two have higher compatibility, can be well fused, plays a skeleton role after the WFB is doped with asphalt, has larger specific surface area of glass fiber in the WFB, and can adsorb a certain amount of oil in the asphalt. The incorporation of WFB improves adsorption between the fibrous asphalt, which in turn improves the technical performance of the matrix asphalt.
Example 2
The preparation method of this example is different from example 1 in that before preparing the modified asphalt of WFB, the WFB is subjected to surface treatment with a silane coupling agent solution, and then the modified asphalt is prepared with the WFB after the surface treatment.
The silane coupling agent has the action mechanism of an organic process of an inorganic filler, and one end of the silane coupling agent is connected with a hydrolyzable X group such as methoxy, ethoxy and the like, as shown in figure 6. According to the characteristics of asphalt, the composition of WFB and the action mechanism of a silane coupling agent, four silane coupling agents such as A-188 (vinyl silane triol triacetate), A-152 (vinyl triacetoxy silane), KH-550 (gamma-aminopropyl triethoxy silane) and KH-792 (diamino silane) are selected.
Three methods are adopted to carry out surface treatment on WFB, and a proper surface treatment mode is explored:
treatment method M1: heating WFB in an oven at 230+ -1deg.C for 1h, cooling, soaking in acetone solution for 1h, taking out, cleaning and air drying; by anhydrous C 2 H 5 Preparing a silane coupling agent solution by OH, fully stirring, standing and hydrolyzing for 10min, and adding quantitative pretreatmentSoaking the WFB for 1h, drying in an oven at 120+/-1 ℃, taking out and cooling for standby.
Treatment method M2: the WFB is put into a stirrer to be stirred slowly, a silane coupling agent solution (which is prepared by absolute ethyl alcohol and is subjected to standing hydrolysis) is slowly added into a container, the higher the rotating speed of the stirrer is, the better the dispersing effect is, the rotating speed is set to 3000r/min, after the instrument is dispersed at high speed for 20min, the container and the material are placed into a baking oven at 120+/-1 ℃ to be dried, and the container and the material are taken out to be cooled for standby.
Treatment method M3: after preparing the silane coupling agent solution and completing hydrolysis, taking a proper amount of WFB, directly putting the WFB into the prepared silane coupling agent solution without treatment, soaking for 1h, then putting into a baking oven at 120+/-1 ℃ for drying, taking out and cooling for later use.
SEM observation of WFB before surface treatment shows that the fibers in WFB are arranged in complicated and staggered manner, and three-dimensional network structure is formed in the space, and the surface of the fibers is not smooth, and particles with different sizes are attached on the surface of the fibers and are in the shape of protruding shell sheets or spheres. In the figure, the particles are identified as resin particles by EDS analysis of an energy spectrum, wherein the main components are C, O and the like. As a result of SEM observation of the WFB after the surface treatment, as shown in fig. 8, a layer of wrapping film was formed on the surface of the WFB by the silane coupling agent, and the silane coupling agent was well bonded to the WFB, but the silane coupling agent was unevenly coated on the fiber surface, forming a sheet film with raised surface. The WFB after treatment was subjected to Mapping surface scanning, and found that the components were mainly Si and O elements, and about 60%, and further, ga, al, na, mg, C and other elements, indicating that the main components were glass fibers and carbon fibers. As shown in FIG. 9, the XRD diffraction patterns of WFB before and after the surface treatment are shown, WFB is amorphous, amorphous substances are relatively large, crystallinity is not strong, and diffraction peaks are not obvious. Comparing X-ray diffraction patterns before and after WFB treatment with silane coupling agent, diffraction peaks appear at 14.04 DEG and 19.80 DEG for both materials, which proves that Al exists in both materials 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The diffraction peak of WFB at 20.52 deg. before and after treatment is SiO 2 Diffraction peak at 26.03℃is B 2 O 3 The diffraction peak at 28.98 ℃may be MgO or Na 2 O, indicating that WFB contains quartz sand, boron-magnesia, etc., i.e., glass fiber groupIn part, both materials show strong diffraction peaks at the same locations in the figure. As a result of corrosion resistance tests on WFB before and after treatment, it was found that the corrosion resistance of WFB treated with a coupling agent solution was improved. The mass loss rate of the WFB is increased along with the increase of the concentration of the NaOH solution and the HCl solution, but the weight loss rate of the WFB after the treatment of the silane coupling agent is improved, and the effect of improving is more obvious as the concentration of the acid-base solution is larger. The agglomeration phenomenon of WFB after the treatment of the silane coupling agent is improved. WFB is softer and more diffuse in texture than acid solutions after corrosion with alkaline solutions.
The contact angle between WFB and asphalt is an important index for visually showing that the wettability of the WFB and the asphalt is good, and the smaller the contact angle is, the better the wettability of the WFB and the asphalt is. The contact angle between WFB treated by silane coupling agent and diiodomethane/deionized water is reduced, and the WFB and nonpolar liquid CH are not treated 2 I 2 The contact angle is 43.4 degrees and the contact angle with deionized water is 99.1 degrees; the contact angle of the treated WFB and diiodomethane becomes 30.3 degrees, the contact angle of the treated WFB and deionized water becomes 87.1 degrees, and the surface energy is 37.95mJ/m 2 Increased to 45.14mJ/m 2 . The surface roughness of the composite fiber is increased, the variety and the number of active groups are increased, and the wettability among the composite fiber liquids is improved after the silane coupling agent is treated.
Referring to the preparation method of the WFB modified asphalt of example 1, the WFB modified asphalt after the silane coupling agent treatment was prepared, and modified asphalt softening point, ductility, penetration, rotational viscosity test was performed, and the results are shown in FIG. 10. The three surface treatment methods M1, M2 and M3 improve the low-temperature ductility value and the softening point value of the WFB modified asphalt to a certain extent, and the difference is small; the viscosity of the WFB modified asphalt after the silane coupling agent treatment is lower than that before the non-treatment, the WFB becomes sticky and hard after the treatment by the methods M2 and M3, and the WFB modified asphalt can generate a splash phenomenon when being mixed with asphalt for high-speed stirring, so that the effect is poor. In summary, the selecting method M1 performs surface treatment on WFB.
The method M1 is adopted to carry out surface treatment on the WFB, the mixing amount of the silane coupling agent in the silane coupling agent solution is 30% of the mass of the WFB, and the proportion of the silane coupling agent solution is as follows: alcohols (ethanol): water=5:85:10, and the influence of different silane coupling agent types on three indexes and viscosity indexes of the modified asphalt is studied.
The test results are shown in FIG. 11, and the WFB modified asphalt treated by four silane coupling agents has unchanged softening point, reduced Brookfield viscosity and increased penetration; the silane coupling agents A-152 and A-188 have obvious low-temperature ductility improvement effect on the modified asphalt, which are respectively improved by 70 percent and 85 percent, and the silane coupling agents AH-550 and AH-792 have smaller influence on the ductility of the modified asphalt. The WFB modified asphalt treated by the silane coupling agent has the advantages of increased fluidity, enhanced tensile strength against external force and slightly increased temperature sensitivity. And comprehensively selecting a silane coupling agent A-188 to carry out surface treatment on the WFB.
Selecting a silane coupling agent A-188, carrying out surface treatment on WFB by adopting a method M1, and determining the doping amount of the silane coupling agent:
the mixing amount of the silane coupling agent A-188 is respectively 15%, 30%, 45%, 60%, 75% and 100% of the mass of the WFB, and the proportion of the silane coupling agent solution is as follows: alcohols (ethanol): water=5:85:10, and the influence of different doping amounts of the silane coupling agent on three indexes and viscosity indexes of the modified asphalt is studied. After the WFB is soaked, WFB modified asphalt is prepared, and three indexes and viscosity indexes are tested, and the results are shown in FIG. 12.
As can be seen from fig. 12, as the blending amount of the silane coupling agent increases, the softening point slightly increases, the penetration value increases, the viscosity decreases, the ductility increases, the 30% solution of the silane coupling agent improves significantly, and the ductility improves by 85%, which means that the silane coupling agent can be well dispersed on the fiber surface. The best combination of the silane coupling agent A-188 is obtained when the mixing amount is 30% of the WFB mass.
FTIR experiments were performed on WFB and WFB modified asphalt before and after silane coupling agent treatment, see fig. 13. As can be seen from FIG. 13, after the silane coupling agent is added, the characteristic absorption peak of Si-O-Si of the WFB is obviously enhanced and the characteristic groups are increased compared with those before treatment, which indicates that the silane coupling agent and the surface of the WFB act to generate new Si-O bonds, the chemical bonding effect is generated, and the affinity with asphalt is better. As can be seen from FIG. 14, the WFB modified asphalt before and after the silane coupling agent treatment has unchanged functional groups, substantially consistent with the absorption peak of the matrix asphalt, and slightly different in strength, which indicates that the WFB treated by the silane coupling agent is incorporated into the matrix asphalt and physically dispersed, and does not have chemical action.
Example 3
The embodiment provides a preparation method of waste fan blade composite fiber and SBS composite modified asphalt, which comprises the following steps:
crushing and screening the WFB, and selecting the WFB with the grain diameter of 0.15-0.3mm for standby;
heating matrix asphalt to a molten state at 145+/-5 ℃, then doping SBS, and stirring for 20min under the condition that the heating temperature is 160-170 ℃ and 2000rad/min to prepare SBS modified asphalt, wherein the doping amount of SBS is 1-4% of the mass of the matrix asphalt;
adding the selected WFB, uniformly stirring, and then placing in a 160+/-1 ℃ oven for thermal insulation swelling for 10min, wherein the doping amount of the WFB is 0.5% -4% of the mass of the SBS modified asphalt;
regulating the temperature of the blend of the SBS modified asphalt and the WFB to 140-160 ℃, and shearing at a high speed of 4000-6000 rad/min for 20-60 min;
and (3) developing the sheared blend of the SBS modified asphalt and the WFB at the constant temperature of 150+/-1 ℃ for 10min to obtain the SBS/WFB compound modified asphalt.
In some embodiments, as shown in fig. 15, the matrix pitch is heated to a molten state at 145 ℃;
adding the selected WFB into the prepared SBS modified asphalt, uniformly stirring, and then carrying out heat preservation and swelling for 10min at 160 ℃;
regulating the temperature of the blend of the SBS modified asphalt and the WFB to 140 ℃, and shearing for 40min at a high speed of 4000 rad/min;
and (3) developing the sheared blend of the SBS modified asphalt and the WFB at the constant temperature of 150 ℃ for 10min to obtain the SBS/WFB compound modified asphalt.
For convenience of description, the SBS blending amount is 1%, the WFB blending amount is 0.5% of the SBS modified asphalt, and the SBS is marked as SBS1-WFB0.5, and the other is the same. The SBS/WFB re-doped modified asphalt is subjected to three-index, 135 ℃ rotational viscosity, segregation, RTFOT and other tests according to the test rules, and the high-temperature stability, low-temperature crack resistance, temperature sensitivity, aging resistance and the like of the re-doped modified asphalt are researched. Main component analysis tests are carried out on SBS/WFB compound modified asphalt with different mixing amounts, and 20 groups of mixing performance indexes are shown in Table 8.
TABLE 8 test results of SBS/WFB multiple blending modified asphalt at different blending amounts
The main component analysis is carried out on the test result by adopting SPSS software, and the SBS/WFB complex blending modified asphalt comprehensive performance score based on the main component analysis is obtained, and is shown in Table 9.
TABLE 9 Main ingredient Synthesis score of SBS/WFB Complex modified asphalt with different blending amounts
As shown in Table 9, when the SBS blending amount is 4% of the mass of the matrix asphalt, the SBS/WFB complex blending modified asphalt has better comprehensive performance. The road performance rule analysis is carried out on SBS/WFB complex doped modified asphalt with different doping amounts.
1. Temperature sensitivity evaluation:
the penetration test was performed on SBS/WFB complex blended modified asphalt at 15, 25, 30℃, and the results are shown in Table 10.
Table 10 results of penetration test of SBS/WFB complex blend modified asphalt
Category(s) Regression equation Correlation coefficient R 2 Penetration index
SBS0-WFB0.5 y=0.0602x+0.1286 0.9996 -2.52
SBS0-WFB1 y=0.0543x+0.2961 0.9974 -1.92
SBS0-WFB2 y=0.0555x+0.2150 0.9993 -2.05
SBS0-WFB4 y=0.0560x+0.1299 0.9998 -2.11
SBS1-WFB0.5 y=0.0545x+0.2660 0.9954 -1.95
SBS1-WFB1 y=0.0491x+0.4075 0.9957 -1.32
SBS1-WFB2 y=0.0459x+0.4751 0.9989 -0.90
SBS1-WFB4 y=0.0461x+0.3954 0.9971 -0.92
SBS2-WFB0.5 y=0.0433x+0.5746 1.0000 -0.52
SBS2-WFB1 y=0.0434x+0.5552 0.9962 -0.54
SBS2-WFB2 y=0.0436x+0.5261 0.9989 -0.57
SBS2-WFB4 y=0.0504x+0.3323 0.9961 -1.48
SBS3-WFB0.5 y=0.0490x+0.3806 0.9944 -1.30
SBS3-WFB1 y=0.0440x+0.5330 0.9995 -0.63
SBS3-WFB2 y=0.0458x+0.4285 0.9998 -0.88
SBS3-WFB4 y=0.0462x+0.3875 1.0000 -0.94
SBS4-WFB0.5 y=0.0525x+0.2839 0.9976 -1.72
SBS4-WFB1 y=0.0458x+0.4590 0.9952 -0.88
SBS4-WFB2 y=0.0428x+0.5118 0.9997 -0.45
SBS4-WFB4 y=0.0430x+0.4720 0.9991 -0.48
As can be seen from FIG. 16, when the SBS blending amount is constant, the penetration P value of the SBS/WFB blended modified asphalt decreases with increasing WFB blending amount, which means that WFB increases the consistency of asphalt and the shear resistance is also improved. Both SBS and WFB improve the temperature sensing properties of the matrix asphalt, with the PVN absolute values of SBS4-WFB4 and SBS4-WFB2 being minimal.
2. High temperature stability evaluation:
as can be seen from FIG. 17, at a constant SBS content, the softening point and 135℃rotational viscosity of the SBS/WFB complex blend modified asphalt increased with increasing WFB content. At a certain SBS doping amount, T 800 Increasing with increasing WFB doping amount; equivalent softening point T when WFB is blended in a certain amount 800 The mixing amount of SBS is increased and then reduced.
3. Low temperature crack resistance:
as can be seen from FIG. 18, when the SBS content is constant, the 15 ℃ ductility of the SBS/WFB complex-blended modified asphalt decreases as the WFB content increases, T 1.2 The trend of firstly decreasing and then increasing along with the increase of the mixing amount of the WFB shows that the WFB can improve the low-temperature performance of asphalt to a certain extent, the WFB generates a tightly-lapped three-dimensional network structure in the asphalt, and plays a good role in inhibiting cracks.
4. Plastic interval:
the temperature difference between the equivalent softening point and the equivalent brittle point of the asphalt is called a plasticity interval delta T, and if the plasticity range of the asphalt is increased, the temperature sensing performance of the asphalt is improved. As can be seen from fig. 19, the plastic interval of the WFB modified asphalt after being mixed with SBS increases, which indicates that the interval from the low temperature embrittlement point to the high temperature softening point of the SBS/WFB re-mixed modified asphalt increases, i.e., the temperature stability interval increases, and the temperature performance of the modified asphalt is more stable.
Storage stability:
as can be seen from FIG. 20, the storage stability of the four groups of SBS/WFB complex-doped modified asphalt meets the segregation softening point difference value of less than or equal to 2.5 ℃ required by the specification, and the reliability of the preparation process is proved.
Ageing resistance:
RTFOT aging tests were performed on four groups of SBS/WFB complex mix modified asphalt, four groups of single mix SBS modified asphalt and four groups of single mix WFB modified asphalt according to test procedure T0610, and the results are shown in Table 11.
Table 11 ageing test index for modified bitumen
As can be seen from Table 11, the mass loss of SBS/WFB complex-doped modified asphalt, single-doped SBS modified asphalt and single-doped WFB modified asphalt are all negative values, and meet the requirement of not more than 0.8% of the specification; the mass loss percentage of the SBS/WFB complex mixing modified asphalt is larger than that of the single mixing SBS modified asphalt and the single mixing WFB modified asphalt. The softening point of the single-doped WFB modified asphalt becomes larger after thermal oxidation, and the increment amplitude of the softening point becomes smaller along with the doping amount of the WFB. The penetration ratio of WFB modified asphalt and SBS modified asphalt is respectively reduced and increased along with the increase of the respective blending amount. Proper amount of WFB is added into SBS modified asphalt to increase penetration ratio and improve ageing resistance of asphalt. The aging indexes of the SBS4-WFB2 and the SBS4-WFB4 are smaller, the viscosity ratio is close to 1, which shows that the higher the high-temperature performance is, the better the aging resistance is, and the low-temperature ductility index after aging is improved to a certain extent. In the four groups of SBS/WFB complex doped modified asphalt, the ductility ratio of the SBS/WFB complex doped modified asphalt is improved along with the increase of the WFB or SBS doping amount at a certain time, and is consistent with a single doping rule.
Microscopic performance:
and (3) carrying out experimental analysis on the sample by utilizing an Atomic Force Microscope (AFM) and software NanoScope Analysis to obtain the three-dimensional microscopic morphology of the asphalt on the nanometer scale, and calculating to obtain the asphalt surface roughness on the basis. The surface roughness is related to the self-healing ability and adhesion properties of asphalt, i.e. the higher the roughness of asphalt, the better the self-healing ability and adhesion properties. As can be seen from FIG. 21, the roughness of the matrix asphalt is larger, and the roughness of the single-blending SBS modified asphalt and the WFB modified asphalt is smaller than that of the matrix asphalt, and SBS4-WFB2 is selected as the optimal blending amount of the multi-blending modified asphalt.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention are included in the protection scope of the present invention.

Claims (2)

1. The preparation method of the waste fan blade composite fiber modified asphalt is characterized by comprising the following steps:
crushing and screening waste fan blades, and selecting waste fan blade crushed materials with the particle size of 0.15-0.3mm and the length of more than 200 mu m as waste fan blade composite fibers, namely WFB;
firstly, adopting a silane coupling agent to carry out surface treatment on the selected WFB, and then adopting the WFB after the surface treatment to prepare modified asphalt;
the WFB was surface treated with a silane coupling agent solution by:
heating WFB in an oven at 230+ -1deg.C for 1h, cooling, soaking in acetone solution for 1h, taking out, cleaning and air drying; then soaking in a silane coupling agent solution for 1h, drying in an oven at 120+/-1 ℃, taking out and cooling for standby;
the mixing amount of the silane coupling agent is 30% of the mass of the selected WFB;
the mass ratio of silane, ethanol and water in the silane coupling agent solution is 5:85:10;
heating the matrix asphalt to a molten state at 145+/-5 ℃, and adding WFB treated by a silane coupling agent into the matrix asphalt in the molten state, wherein the addition amount of the WFB is 2% of the mass of the matrix asphalt;
developing for 30min at the constant temperature of 160+/-1 ℃, and stirring the WFB and matrix asphalt mixture for thermal insulation swelling;
high-speed shearing is carried out on the mixture of the WFB and the matrix asphalt after swelling at the temperature of 140 ℃, the shearing rate is 4000r/min, and the shearing time is 40min;
and (3) keeping the temperature of the sheared blend of the WFB and the matrix asphalt at 145+/-1 ℃ for 10min to obtain the WFB modified asphalt.
2. The method for preparing the waste fan blade composite fiber modified asphalt according to claim 1, wherein when the WFB treated by the silane coupling agent is added to the matrix asphalt in a molten state, the WFB is added in 3 times under the conditions of heating and stirring.
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CN111233374A (en) * 2020-01-20 2020-06-05 河北安恕朗晴环保设备有限公司 Asphalt mastic macadam mixture using recycled fan blade waste as filler
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