CN103710040A - Lignin modified asphalt, preparation method therefor and applications thereof - Google Patents
Lignin modified asphalt, preparation method therefor and applications thereof Download PDFInfo
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- CN103710040A CN103710040A CN201310647897.2A CN201310647897A CN103710040A CN 103710040 A CN103710040 A CN 103710040A CN 201310647897 A CN201310647897 A CN 201310647897A CN 103710040 A CN103710040 A CN 103710040A
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- xylogen
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Abstract
Provided are a kind of lignin modified asphalt, a preparation method therefor and applications thereof. The modified asphalt is prepared after the following steps: first, lignin extraction is carried out; second, lignin refining is carried out; third, lignin modification is carried out; fourth, the modified lignin obtained from the third step and petroleum asphalt are placed in a reaction vessel, Na2S is added, the reaction is for 30min, and lignin modified asphalt is obtained after postprocessing. In the method, lignin is extracted from waste papermaking black liquid, asphalt is subjected to chemical modification by utilization of lignin after refining and modification, and lignin modified asphalt is obtained. The corrosion resistance of the modified asphalt is comparable to that of asphalt before modification, the elastic recovery rate of the modified asphalt is higher than that of asphalt before modification by 1.2%, the viscosity of the modified asphalt is higher than that of asphalt before modification at the same temperature, and therefore the performances of the modified asphalt is comparable to that of unmodified asphalt, so asphalt can be replaced by the lignin modified asphalt, not only petroleum resource is saved but also secondary utilization of waste papermaking black liquid is achieved.
Description
Technical field
The invention belongs to environmental engineering research field, be specifically related to a kind of lignin modified asphalt and its preparation method and application.
Technical background
Pitch plays an important role in the construction of road, and the pitch that China is used is mostly from the byproduct of oil, and oil is Nonrenewable resources, to the demand of pitch is increasing, will further cause the shortage of petroleum resources.
On the other hand, a large amount of black liquid of the annual generation of the papermaking industry of China, if appropriate not to the processing of black liquid, can make a big impact to environment.
In sum, the environmental pollution causing in order to save the improvement black liquid of petroleum resources and science, the modification that black liquid is rationally used in to pitch has important social value.At present, the research of China to lignin modified asphalt, is also only in the aspect of the basic physically modified such as even blend degree, intensity and temperature variation of xylogen and pitch, does not carry out the research of xylogen to the chemical modification of pitch.
In order to address the above problem, the present invention be take lignin polymers and bituminous matter as basis, utilizes the xylogen extracting in black liquid to carry out chemical modification to pitch.
Summary of the invention
The technical problem solving is: the present invention overcomes the deficiencies in the prior art and proposes a kind of lignin modified asphalt and its preparation method and application, utilize the lignin modified asphalt that the method prepares to there is good corrosion resistance, elastic recovery capability and viscosity, alternative petroleum pitch.
Technical scheme:
Lignin modified asphalt, by following steps, prepare and obtain:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 2.5-3.5, and the black liquid of acidifying is warming up to 80 ℃ in 15-20min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 15-25 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 1.5-2.5 with salt acid for adjusting pH, at 70-90 ℃, stirs after 2.5-3.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 0.5-1.5h at 70-90 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 2.5-3.5h, with the pH value of hydrochloric acid conditioning solution, be 1.5-2.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:(50-125): (3-5): 5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 350-400 ℃, 20-25MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is (3-5): (5-7): (3-4): 20.
The preparation method of described lignin modified asphalt, comprises the steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 2.5-3.5, and the black liquid of acidifying is warming up to 80 ℃ in 15-20min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 15-25 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 1.5-2.5 with salt acid for adjusting pH, at 70-90 ℃, stirs after 2.5-3.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 0.5-1.5h at 70-90 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 2.5-3.5h, by the pH value of hydrochloric acid conditioning solution, be 1.5-2.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:(50-125): (3-5): 5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 350-400 ℃, 20-25MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is (3-5): (5-7): (3-4): 20.
The preparation method of described lignin modified asphalt is warming up to 80 ℃ by the black liquid of acidifying in step (1) in 18min.
The preparation method of described lignin modified asphalt, the temperature of reaction in step (2) is 80 ℃, the time is 3h.
The preparation method of described lignin modified asphalt, the mass ratio of refining xylogen in step (3), 5% NaOH solution, epoxy chloropropane, ethanol is 1:100:4:5.
The preparation method of described lignin modified asphalt, the temperature of reaction in step (4) is 375 ℃, pressure is 22.1MPa.
The application of lignin modified asphalt in Road construction.
In step of the present invention (4), at basic metal (Na
﹢or K
﹢) under the effect of catalyzer, Na
2ionic linkage fracture in S, the phenolic hydroxyl group existing in lignin molecule structure and alcoholic extract hydroxyl group isoreactivity group make the molecule in xylogen and bituminous matter complete sulfonation, form C-S key, C-S key is by different together molecule crosslinked, therefore alkali lignin and petroleum pitch fully can be merged.
Beneficial effect: the present invention is from discarded extracting lignose from papermaking black liquor, and utilize the xylogen after refining modification to carry out chemical modification to pitch, obtain lignin modified asphalt, before the corrosion resistance of modifying asphalt and modification, pitch is suitable, its elastic restoration ratio compared with modification before pitch high by 1.2%, its viscosity is at the same temperature higher than the viscosity of unmodified front pitch, therefore the performance of lignin modified asphalt and unmodified pitch is suitable, therefore available lignin modified asphalt replaces pitch, both petroleum resources had effectively been saved, again discarded black liquid has been carried out to second stage employ.
Embodiment
Embodiment 1:
The preparation method of lignin modified asphalt, comprises the steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 3.5, and the black liquid of acidifying is warming up to 80 ℃ in 15min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 15 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 2.5 with salt acid for adjusting pH, at 70 ℃, stirs after 3.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 1.5h at 70 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 3.5h, by the pH value of hydrochloric acid conditioning solution, be 2.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:50:3:5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 350 ℃, 20MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is 3:7:3:20.
Embodiment 2:
The preparation method of lignin modified asphalt, comprises the steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 2.5, and the black liquid of acidifying is warming up to 80 ℃ in 20min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 25 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 1.5 with salt acid for adjusting pH, at 90 ℃, stirs after 2.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 0.5h at 90 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 2.5h, by the pH value of hydrochloric acid conditioning solution, be 1.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:125:5:5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 400 ℃, 25MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is 5:5:4:20.
Embodiment 3:
The preparation method of lignin modified asphalt, comprises the steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 3, and the black liquid of acidifying is warming up to 80 ℃ in 18min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 20 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 2 with salt acid for adjusting pH, at 80 ℃, stirs after 3h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 1h at 80 ℃, adds the ethanolic soln of epoxy chloropropane in reactor, reaction 3h, by the pH value of hydrochloric acid conditioning solution, be 2, suction filtration is got filter cake, with deionized water, is repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:100:4:5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 375 ℃, pressure is 22.1MPa, and stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is 4:6:3:20.
The lignin modified asphalt that embodiment 3 is made carries out acid rain corrosion weathering test, recovery of elasticity test and viscosity test:
One, acid rain corrosion weathering test
Respectively the lignin modified asphalt of three groups of 3.850g is dissolved in 10ml trieline, and pour in the thin film oven platter that diameter is 14cm, after volatilizing completely, trieline obtains the asphalt membrane sample of 250 μ m thickness, three asphalt membranes are tiled respectively it is fully immersed in three furnace potes, within every 24 hours, add 37% hydrochloric acid soln, respectively pH is adjusted to 1.0,3.0 and 5.6, every 24h sampling once, test period is 240h, and water is cleaned remaining pitch, dries, weigh, quality is X(g).Utilize formula ((3.85-X) ÷ 3.85) * 100, calculate the rate that the is corroded p (%) of pitch.
The results are shown in Table 1.
Table 1 lignin modified asphalt and unmodified pitch residual volume and the rate that is corroded after acid corrosion
As shown in Table 1, under identical pH value, the degree that is corroded of lignin modified asphalt and petroleum pitch is almost equal, even a little higher than petroleum pitch of the resistance to corrosion of lignin modified asphalt.As can be seen here, by xylogen, pitch is carried out to chemical modification, pitch after modification has good resistance to corrosion, therefore utilize the xylogen extracting from black liquid to carry out modification to common petroleum pitch, the alternative unmodified pitch of pitch obtaining, has not only saved petroleum resources but also take full advantage of black liquid waste.
Two, recovery of elasticity test
Recovery of elasticity test is for measuring and evaluate modifying asphalt under the effect of external force, the ability of recoverable deformation.For modifying asphalt, this is an important evaluation index, and testing method is T0662.Adopt ductility test die trial used, but middle portion is changed to straight line side form, during test, pressing ductility test method rate of extension with 5 scholar 0.25cm/min under test temperature stretches, the length of measuring test specimen is X(cm), ductility test instrument elongate to the percentage of the recoverable deformation after 10cm be elastic restoration ratio, elastic restoration ratio calculation formula: ((10 1 X) ÷ 10) x100
In formula: the remaining lengths of X-sample, cm
Respectively to the tensile elongation of xylogen pitch and common petroleum pitch be 10.02,10.01,9.99cm measures.Measuring result sees the following form 2.
The elastic restoration ratio of table 2 lignin modified asphalt and unmodified pitch
As shown in Table 2, the elastic restoration ratio of lignin modified asphalt in the time of 25 ℃ is higher by 1.2% than plain asphalt, therefore utilize the xylogen extracting from black liquid to carry out modification to common petroleum pitch, the modifying asphalt obtaining can reach the elastic restoration ratio of common petroleum pitch, and then can replace petroleum pitch.
Three, viscosity
China < < highway engineering pitch and Asphalt Mixture Experiment rules > > (JTJ052 1) according to measure pitch from lesser temps to comparatively high temps within the scope of the needs of viscosity; dissimilar viscometer is stipulated respectively; for example; the kinetic viscosity of using for measuring 60 ℃ of viscosity chassifications of pitch, all unifies to adopt vacuum decompression capillary viscosimeter (rules T0620) in the world; The kinematic viscosity of measuring 135 ℃ or higher temperature to determining construction temperature adopts the reverse-flow kapillary method of T0619, the saybolt viscosimeter method of T0623 conventionally.Not (Brookfield) viscometer method (ASTMD4402) of Bu Luoke Field is released in U.S. SHRP plan, can measure 60 ℃ of above kinetic viscosities of pitch and modifying asphalt.This instrument occupies nearly 90% share at home on like product market, and domestic most universities and highway communication Graduate School of Engineering and other unit are all used the kinetic viscosity of this Instrument measuring pitch.
Adopt Brookfield rotary viscometer mensuration lignin modified asphalt and petroleum pitch 100-135 ℃ of temperature field kinetic viscosity, object is to determine the viscosity number of pitch at boiling test temperature.In order to reduce systematic error, the unified rotating speed that adopts 20r/min of test, result is as shown in table 3:
The kinetic viscosity of table 3 lignin modified asphalt and unmodified pitch (Pas)
As shown in Table 3, xylogen pitch viscosity is at the same temperature slightly larger than petroleum pitch.And it is generally acknowledged that kinetic viscosity is the reflection pitch optimal index of resistance toheat in season in full summer, the pitch that viscosity is larger produces less shearing strain under loading action, elastic recovery properties is good, and residual permanent plastic deformation is little, i.e. the ability of road surface opposing rut is strong.Therefore utilize the xylogen extracting from black liquid to carry out modification to common petroleum pitch, the modifying asphalt obtaining has good viscosity.
Therefore, utilize the lignin modified asphalt of the inventive method manufacture to meet the engineering demand of common petroleum pitch completely, alternative unmodified pitch, has not only saved petroleum resources but also take full advantage of black liquid waste.
The application of lignin modified asphalt in Road construction: utilize the produced lignin modified asphalt of this programme can replace common petroleum pitch, for laying road.In addition, due to the content reduction of pitch, its organic amount volatilizing reduces relatively, to the harm of HUMAN HEALTH and farm crop, can greatly reduce.
The invention provides a kind of lignin modified asphalt and preparation method thereof; above-mentioned case study on implementation all can only think explanation of the present invention can not limit the present invention; can also make some improvements and modifications under the premise without departing from the principles of the invention, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. lignin modified asphalt, is characterized in that being prepared and being obtained by following steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 2.5-3.5, and the black liquid of acidifying is warming up to 80 ℃ in 15-20min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 15-25 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 1.5-2.5 with salt acid for adjusting pH, at 70-90 ℃, stirs after 2.5-3.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 0.5-1.5h at 70-90 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 2.5-3.5h, by the pH value of hydrochloric acid conditioning solution, be 1.5-2.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:50-125:3-5:5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 350-400 ℃, 20-25MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is 3-5:5-7:3-4:20.
2. the preparation method of lignin modified asphalt claimed in claim 1, is characterized in that comprising the steps:
(1) extraction of xylogen
Get black liquid, adding salt acid for adjusting pH is 2.5-3.5, and the black liquid of acidifying is warming up to 80 ℃ in 15-20min, by centrifugation, gets lower sediment, and with deionized water repetitive scrubbing, to neutral, at 120 ℃, dry 24h, obtains xylogen crude product;
(2) xylogen is refining
The xylogen crude product of step (1) gained is added to the water, the quality of water is 15-25 times of xylogen crude product, the preparation xylogen aqueous solution, the xylogen aqueous solution preparing is placed in to reactor, is 1.5-2.5 with salt acid for adjusting pH, at 70-90 ℃, stirs after 2.5-3.5h, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtains refining xylogen;
(3) modification of xylogen
It is in 5% NaOH solution that the refining xylogen that step (2) is obtained is dissolved in mass concentration, be placed in reactor, stirring reaction 0.5-1.5h at 70-90 ℃, the ethanolic soln of epoxy chloropropane is added in reactor, reaction 2.5-3.5h, by the pH value of hydrochloric acid conditioning solution, be 1.5-2.5, suction filtration is got filter cake, with deionized water, be repeatedly washed till neutrality, dry 24h in 120 ℃ of baking ovens, obtain modified lignin resin, wherein the mass ratio of refining xylogen, 5% NaOH solution, epoxy chloropropane, ethanol is 1:50-125:3-5:5;
(4) lignin modified asphalt
Modified lignin resin and petroleum pitch that step (3) is obtained are placed in reaction vessel, add Na
2s, at 350-400 ℃, 20-25MPa, stopped reaction after reaction 30min, is cooled to room temperature, adds deionized water, crosses leaching filter cake, and at 120 ℃, dry 24h, obtains lignin modified asphalt, wherein modified lignin resin, petroleum pitch, Na
2the mass ratio of S, deionized water is 3-5:5-7:3-4:20.
3. the preparation method of lignin modified asphalt as claimed in claim 2, is characterized in that, in step (1), the black liquid of acidifying is warming up to 80 ℃ in 18min.
4. the preparation method of lignin modified asphalt as claimed in claim 2, is characterized in that the temperature of reaction in step (2) is 80 ℃, and the time is 3h.
5. the preparation method of lignin modified asphalt as claimed in claim 2, is characterized in that the mass ratio of refining xylogen in step (3), 5% NaOH solution, epoxy chloropropane, ethanol is 1:100:4:5.
6. the preparation method of lignin modified asphalt as claimed in claim 2, is characterized in that the temperature of reaction in step (4) is 375 ℃, and pressure is 22.1MPa.
7. the application of lignin modified asphalt claimed in claim 1 in Road construction.
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| CN111492014A (en) * | 2017-11-13 | 2020-08-04 | 瓦赫宁根基础研究所 | Lignin biological asphalt |
| CN113683899A (en) * | 2021-09-02 | 2021-11-23 | 程小冬 | High-strength high-viscosity asphalt and preparation method thereof |
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| CN111492014A (en) * | 2017-11-13 | 2020-08-04 | 瓦赫宁根基础研究所 | Lignin biological asphalt |
| CN107987621A (en) * | 2017-12-15 | 2018-05-04 | 安徽五岳松纳米技术有限公司 | A kind of aging resistant coating |
| CN113683899A (en) * | 2021-09-02 | 2021-11-23 | 程小冬 | High-strength high-viscosity asphalt and preparation method thereof |
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