CN103804925A - Modified asphalt and preparation method thereof - Google Patents
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- CN103804925A CN103804925A CN201210439802.3A CN201210439802A CN103804925A CN 103804925 A CN103804925 A CN 103804925A CN 201210439802 A CN201210439802 A CN 201210439802A CN 103804925 A CN103804925 A CN 103804925A
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Abstract
The invention discloses a modified asphalt and a preparation method thereof. The modified asphalt comprises the following components by weight: 74%-97% of base asphalt, 0.5%-10% of an additive A, 1.5%-12% of an additive B, and 0.5%-4% of an additive C. Specifically, the base asphalt is petroleum asphalt, the additive A is an aromatic hydrocarbon-rich component, the additive B is one or more of organic acids, and the additive C is an alkali inorganic substance. The preparation method comprises: (1) mixing the part of the base asphalt, the additive A and the additive B evenly; (2) adding the additive C into the mixture obtained in step (1) to conduct saponification reaction, and then raising the temperature to vaporize water; and (3) adding the rest base asphalt into the mixture obtained in step (2), and mixing the materials evenly to obtain the modified asphalt product. The modified asphalt provided by the invention has good high temperature stability, aging resistance and temperature susceptibility, and can be widely used in different areas to build high grade highways of different mixture types.
Description
Technical field
The present invention relates to a kind of modifying asphalt and preparation method thereof, relate in particular to a kind of modifying asphalt of preparing by chemical reaction and method.
Background technology
Due to the difference of region, some area winter, summer temperature difference are larger, bituminous pavement environment for use is severe, in addition the increasing sharply of the volume of traffic, vehicle maximize, the reason such as vehicle heavy duty overload, bituminous pavement occurs that the phenomenons such as high temperature rut, cold cracking and Moisture Damage are still more serious.At present, in heavy duty road asphalt product, majority exists high temperature viscosity and penetrative index is less than normal, the defects such as penetration ratio is little after film heating, be that high-temperature behavior, ageing resistance and temperature sensibility are poor, thereby, be unfavorable for reducing pavement track and gather around the generation of the diseases such as bag and pitch rapid ageing and cause the generation of the too early breakoff phenomenon in road surface.Also often occur causing the phenomenon of peeling off in early days because of pitch and building stones poor adhesion.In addition,, for some crude oil formed asphalt, there is the deficiency that wax content is higher, ductility is less, and can not produce the heavy traffic paving asphalt product that meets index request.
In order to improve high temperature performance and the temperature sensibility of pitch, further improve the use properties of pitch, conventionally adopting more method is in pitch, to add a certain amount of macromolecule polymer material, as styrene-butadiene-styrene block copolymer (SBS), polyethylene (PE) and polypropylene etc., can improve to a certain extent the use propertieies such as the high temperature performance of pitch.Also the method for useful atmospheric oxidation or catalyzed oxidation improves the technique of pitch high temperature performance.
The patent such as CN101962482A and CN1569964A is to utilize the modifying asphalt technology of preparing of SBS as properties-correcting agent.CN1523050A and CN101200596A utilize the modifying asphalt technology of preparing of SBR as properties-correcting agent.Although have certain modified effect, macromolecular material is expensive, and production unit is required strictly, production technique is more complicated, and comprehensive process cost is higher.CN101974235A is a kind of wide territory modifying asphalt technology of preparing, using Powdered styrene-butadiene rubber(SBR) as the first properties-correcting agent, using polyethylene wax as the second properties-correcting agent, by high-melting-point and the above characteristic of melting fast of fusing point of polyethylene wax, make modifying asphalt possess the performance of certain polyethylene wax, improve the softening temperature of pitch, utilize the low temperature deep drawing quality energy of styrene-butadiene rubber(SBR), the low temperature extensibility of modifying asphalt is increased, belong to physically modified category, not only cost is higher, and have problems with the consistency of pitch, while being thermmal storage, once stop stirring, there will be demixing phenomenon.
CN1487029A carries out modification to pitch jointly with rock asphalt and organo-metallic soap and powder styrene butadiene rubber.CN1587320A with in CN1837292A, be with wilkinite, silicate or diatomite etc. together with powder styrene butadiene rubber to asphalt modification, and styrene-butadiene rubber(SBR) is the main body of properties-correcting agent, belong to by adding some additive to prepare styrene-butadiene rubber(SBR) composite modified asphalt technology.Exist equally and increase the deficiency such as cost, easy laminated segregation.
CN1178822A provides a kind of preparation method of oxidized bitumen, although the method can be improved the use properties such as high temperature performance and temperature sensibility of pitch, but due to oxidizing process relative complex, and can pollute air, to such an extent as to be restricted on actual use.
US4874432 and CN102558887A disclose respectively a kind of multistage pitch preparation process and gel modified asphalt preparation technology.The saponification process of the two is basically identical, and by adding the Yatall MA (being tall oil) that contains lipid acid and resinous acid and solid water-free alkali metal base to carry out saponification reaction in pitch, difference is also to have added in CN102558887A amine or acid amides.Two pieces of patents, in not reducing pitch low-temperature performance, have improved high temperature performance of asphalt.But also there are the following problems: saponification reaction speed and reactant concn are proportional, concentration is too little is unfavorable for that reaction normally carries out, and directly Yatall MA and alkali is joined in whole pitch, because saponifiable matter concentration is low, can greatly reduce speed of response, generally the more difficult saponification reaction of carrying out well.
Summary of the invention
The invention provides a kind of have good temperature sensibility, cost is low, character is good modifying asphalt, the invention provides simple, the easy to operate process for preparing modified asphalt of a kind of complete processing simultaneously.
Modifying asphalt of the present invention, comprises following component in modifying asphalt mass percent:
(1) basic asphalt 74%～97%; Be preferably 79.5%～92%;
(2) additive A 0.5%～10%; Be preferably 2%～8%;
(3) additive B 1.5%～12%; Be preferably 4%～10%;
(4) addition of C 0.5%～4%; Be preferably 1.5%～2.5%.
Wherein basic asphalt is petroleum pitch, comprises the de-oiled asphalt that vacuum residuum, straight-run pitch, solvent de-asphalting process obtain, one or more that are in harmonious proportion in pitch and oxidized bitumen.25 ℃ of penetration degrees of basic asphalt are 40～300 1/10mm, are preferably 50～200 1/10mm.The softening temperature of basic asphalt is 25～70 ℃, is preferably 35～65 ℃.
Additive A is for being rich in aromatic component, derives from one or more the mixture in extraction oil, catalytically cracked oil, the vacuum distillate of naphthenic base crude and the used oil of recovery of lubricating oil solvent, the preferably extraction oil of lubricating oil solvent.
Additive B is one or more in organic acid, includes but not limited to animal, plant fatty acid, as stearic acid (18 carbonic acid), ten dihydroxystearic acids etc., also comprises C
10~ C
18synthetic fatty acid, preferably C
14~ C
18synthetic fatty acid.
Addition of C mainly comprises bases inorganics, as one or more in the inorganic additivess such as sodium hydroxide, lithium hydroxide, potassium hydroxide and calcium hydroxide.
In modified asphalt composite of the present invention, can also add as required other additive, as organic substances such as glycerol, rosin and naphthenic acid, its add-on generally accounts for 0.5%～5% of modifying asphalt quality.
The preparation method of modified asphalt composite of the present invention, comprises following content: (1) mixes part basic asphalt, additive A and additive B; (2) in the mixture obtaining to step (1), add addition of C, react, transpiring moisture then heats up; (3) remaining basic asphalt is added in the mixture that step (2) obtains, mix, obtain modifying asphalt product.
In the inventive method, the temperature of basic asphalt is 100～170 ℃, preferably 110～160 ℃, the temperature of additive A is 50～120 ℃, step (1) adds 20wt%～40wt% basic asphalt, the mixing time of step (1) is 10～90 minutes, and mixing temperature is 90～150 ℃, preferably 20～60 minutes.
In the inventive method step (2), temperature of reaction is 90～150 ℃, and the reaction times is 0.5～8 hour, preferably 1～5 hour; And then heat up 30～90 ℃, moisture is evaporated in mixture without bubble.
In the inventive method step (3), mixing time is 20～180 minutes, and mixing temperature is 120～280 ℃.
The inventive method can also add one or more in glycerol, rosin or naphthenic acid in step (1) and/or step (2) as required, and its add-on generally accounts for 0.5%～5% of modifying asphalt quality.
The inventive method step (3) optimal way is: remaining basic asphalt is added in the mixture that step (2) obtains, with 30～120 minutes, stir and be warming up to 160～280 ℃, preferably 180～260 ℃, mix.
The inventive method adopts common whipping device or high-shear to be uniformly mixed.
In the inventive method, addition of C adds in the mode of bases aqueous solution of inorganic matter or water miscible liquid, wherein the concentration of sodium hydroxide and potassium hydroxide aqueous solution is 20wt% ~ saturated solution, lithium hydroxide aqueous solution concentration is 10wt% ~ saturated solution, and calcium hydroxide is 20wt% ~ 30wt% water miscible liquid.
In the inventive method, basic asphalt and additive A preferably do not contain moisture, in case there is the still phenomenon of overflowing.The object that adds additive A is to reduce the viscosity of pitch, for subsequent reactions provides a suitable place.
Modifying asphalt of the present invention has good high-temperature stability, ageing resistance and temperature sensibility, can be widely used in different areas and build the high-grade highway of different mix type, is specially adapted to build the high-grade highway in high temperature area.
The inventor finds under study for action, directly in pitch medium, add the highly basic such as solid sodium hydroxide, because solid alkali disperses inhomogeneous in pitch, can make saponification reaction be difficult to fully carry out, and saponification reaction product is soap class and water, temperature of reaction is more than 190 ℃, and the water that reaction produces, at this temperature, very easily causes the still and cannot normal running of overflowing when rapid evaporation.
Compared with prior art, tool of the present invention has the following advantages:
(1) adopting organic acid, synthetic fatty acid and rosin etc. is raw material, can adjust according to actual needs and control raw material composition, and then effectively guarantees the performance of modifying asphalt.
(2) alkali that reaction is used adds with the form of alkali aqueous solution and water miscible liquid, and alkali is dispersed in pitch medium, thereby impels reaction to carry out fast.
(3) in reaction process, add the fragrant component of a small amount of richness and part basic asphalt, but not whole basic asphalts, when reducing dielectric viscosity, increase the concentration of saponification reaction thing, be conducive to react at lower temperature, improve speed of response, be unlikely to again to make to add and react the water producing rapid evaporation causes the generation of excessive still phenomenon because temperature is high.
(4) in reaction process, add synthetic fatty acid, naphthenic acid and rosin, meet alkali and react, be conducive to the initial stage milk sap that System forming is fine, thus fast reaction speed.
(5) modifying asphalt of the present invention has softening temperature and high temperature viscosity is moderate, the features such as penetrative index is larger, as the modifying asphalt of penetration degree 40-100 1/10mm, more than its 60 ℃ of kinematic viscosity can reach 300Pa.s, penetrative index is more than 1.0, and ageing index is below 2.0.
Embodiment
Below will by embodiment, the present invention will be further described, percentage ratio is wherein mass percent.
Embodiment 1
The straight-run pitch of 47.0 ℃ of 25 ℃ of penetration degree 70 1/10mm, softening temperature is heated to 150 ℃ of meltings, taking 200g basic asphalt is contained in the metal vessel that volume is 1000ml, add the lube oil finishing of 50g80 ℃ to extract oil out, it is mixed with common whipping device, then add 40g stearic acid (secondary), stir and within 30 minutes, make it melt to mix, at 105 ℃, slowly adding concentration is 30% aqueous sodium hydroxide solution 21g.And continue to stir 2.5 hours, be then warming up to 160 ℃, when without bubble, add again the basic asphalt of 400g160 ℃, and after being fully uniformly mixed, can test the character (the results are shown in Table 1) of modifying asphalt.
Embodiment 2
The straight-run pitch of 45.8 ℃ of 25 ℃ of penetration degree 100 1/10mm, softening temperature is heated to 150 ℃ of meltings, taking 180g basic asphalt is contained in the metal vessel that volume is 1000ml, add the lube oil finishing of 45g80 ℃ to extract oil out, it is mixed with common whipping device, then add 35g stearic acid (secondary) and 15g rosin (one-level), stir and within 40 minutes, make it melt to mix, at 105 ℃, slowly adding concentration is 30% aqueous sodium hydroxide solution 25g.And continue to stir 2 hours, then be warming up to 160 ℃, when without bubble, add again the basic asphalt of 420g160 ℃, be uniformly mixed with common agitation mixer, be warming up to 250 ℃ with the time of approximately 60 minutes simultaneously, while being then cooled to 170 ℃, can test the character (the results are shown in Table 1) of modifying asphalt.
Embodiment 3
The blend asphalt of 49.2 ℃ of 25 ℃ of penetration degree 60 1/10mm, softening temperature is heated to 160 ℃ of meltings, taking 180g basic asphalt is contained in the metal vessel that volume is 1000ml, add the lube oil finishing of 30g80 ℃ to extract oil out, it is mixed with common whipping device, then add 30g stearic acid (secondary) and 15g synthetic fatty acid (C
14~ C
18), stir and within 20 minutes, make it melt to mix, at 105 ℃, slowly adding concentration is 30% aqueous sodium hydroxide solution 24g.And continue to stir 3 hours, then be warming up to 160 ℃, when without bubble, add again the basic asphalt of 420g160 ℃, be uniformly mixed with common agitation mixer, be warming up to 260 ℃ with the time of approximately 80 minutes simultaneously, while being then cooled to 170 ℃, can test the character (the results are shown in Table 1) of modifying asphalt.
Embodiment 4
The straight-run pitch of 39.7 ℃ of 25 ℃ of penetration degree 160 1/10mm, softening temperature is heated to 160 ℃ of meltings, taking 200g basic asphalt is contained in the metal vessel that volume is 1000ml, add 40g80 ℃ subtract four line distillates (Zhenghai refinery product), with common whipping device stirring 30 minutes, then add 49g ten dihydroxystearic acids and 21g stearic acid, stir and within 30 minutes, make it melt to mix, at 110 ℃, slowly adding concentration is 10% lithium hydroxide 86g.And continue to stir 3 hours, then be warming up to 140 ℃, when without bubble, add again the basic asphalt of 410g160 ℃, be uniformly mixed, be warming up to 230 ℃ with the time of approximately 60 minutes simultaneously, while being then cooled to 160 ℃, can test the character (the results are shown in Table 1) of modifying asphalt.
Embodiment 5
The straight-run pitch of 46.7 ℃ of 25 ℃ of penetration degree 90 1/10mm, softening temperature is heated to 160 ℃ of meltings, taking 200g basic asphalt is contained in the metal vessel that volume is 1000ml, add the lube oil finishing of 25g80 ℃ to extract oil out, it is mixed with common whipping device, then add 45g stearic acid (secondary) and 15g glycerol, stir and within 30 minutes, make it melt to mix, at 110 ℃, slowly adding concentration is 30% aqueous sodium hydroxide solution 23.5g.And continue to stir 2.5 hours, be then warming up to 160 ℃, when without bubble, add again the basic asphalt of 400g160 ℃, and be under agitation warming up to 220 ℃, while being then cooled to 170 ℃, can test the character (the results are shown in Table 1) of modifying asphalt.
Comparative example 1
By asphalt heating to 200 used ℃ melting in embodiment 1, taking this pitch of 500g is contained in the metal vessel that volume is 750ml, in shearing grinding with high-shear machine, add in the sodium hydrate particle and pitch that 1.3g is dry, continue to shear 2 minutes, add paper mill, the Yalu River, 10g Dandong to produce Yatall MA, and continue shear-mixed 20 minutes, cannot carry out analytical test owing to still having a large amount of foams, therefore the baking oven relaying continuation of insurance that sample is put into 150-160 ℃ is held 20 minutes, stir and make foam reduce rear sampling analysis asphaltic nature (the results are shown in Table 1) with glass stick simultaneously.
Comparative example 2
By asphalt heating to 200 used ℃ melting in embodiment 1, taking this pitch of 500g is contained in the metal vessel that volume is 750ml, in shearing grinding with high-shear machine, add in the lithium hydroxide particle and pitch that 1.3g is dry, continue to shear 2 minutes, add paper mill, the Yalu River, 10g Dandong to produce Yatall MA, and continue shear-mixed 20 minutes, cannot carry out analytical test owing to still having a large amount of foams, therefore the baking oven relaying continuation of insurance that sample is put into 150-160 ℃ is held 20 minutes, be stirred to foam with glass stick simultaneously and reduce rear sampling analysis asphaltic nature (the results are shown in Table 1).
Table 1 modified bitumen product character.
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 |
| Penetration degree (25 ℃)/0.1mm | 56 | 72 | 50 | 96 | 67 | 50 | 49 |
| Softening temperature/℃ | 59.5 | 61.2 | 64.8 | 54.7 | 64.1 | 54.3 | 55.6 |
| Viscosity (60 ℃)/Pa.s | 311.2 | 351.4 | 419.7 | 307.0 | 344.9 | 312.4 | 335.3 |
| Penetrative index | 1.22 | 2.27 | 1.94 | 1.76 | 2.62 | 0.04 | 0.06 |
| Thin Film Oven Test TFOT (163 ℃, 5h) | ? | ? | ? | ? | ? | ? | ? |
| Penetration ratio/% | 81.4 | 84.9 | 86.7 | 80.9 | 82.6 | 78.9 | 81.2 |
| Ageing index | 1.67 | 1.48 | 1.52 | 1.59 | 1.32 | 2.36 | 2.05 |
As can be seen from the above data, modifying asphalt softening temperature and penetrative index that the inventive method obtains are larger, and ageing index is less, has the advantages such as good temperature sensibility, high-temperature behavior and resistance to deterioration.
Claims (14)
1. a modifying asphalt, is characterized in that: comprise following component in modifying asphalt mass percent:
(1) basic asphalt 74%～97%;
(2) additive A 0.5%～10%;
(3) additive B 1.5%～12%;
(4) addition of C 0.5%～4%;
Wherein basic asphalt is petroleum pitch, and additive A is for being rich in aromatic component, and additive B is one or more in organic acid, and addition of C is bases inorganics.
2. according to modifying asphalt claimed in claim 1, it is characterized in that: comprise following component in modifying asphalt mass percent:
(1) basic asphalt 79.5%～92%;
(2) additive A 2%～8%;
(3) additive B 4%～10%;
(4) addition of C 1.5%～2.5%.
3. according to modifying asphalt claimed in claim 1, it is characterized in that: described basic asphalt is the de-oiled asphalt that obtains of vacuum residuum, straight-run pitch, solvent de-asphalting process, one or more that are in harmonious proportion in pitch and oxidized bitumen, 25 ℃ of penetration degrees of basic asphalt are 40～300 1/10mm, and softening temperature is 25～70 ℃.
4. according to modifying asphalt claimed in claim 1, it is characterized in that: described additive A derives from one or more the mixture in extraction oil, catalytically cracked oil, the vacuum distillate of naphthenic base crude and the used oil of recovery of lubricating oil solvent.
5. according to modifying asphalt claimed in claim 1, it is characterized in that: described additive B is animal, plant fatty acid and C
10~ C
18synthetic fatty acid in one or more.
6. according to modifying asphalt claimed in claim 1, it is characterized in that: described addition of C is one or more in sodium hydroxide, lithium hydroxide, potassium hydroxide and calcium hydroxide.
7. according to modifying asphalt claimed in claim 1, it is characterized in that: in modified asphalt composite, add one or more in glycerol, rosin and naphthenic acid, its add-on accounts for 0.5%～5% of modifying asphalt quality.
8. a preparation method for modifying asphalt claimed in claim 1, is characterized in that comprising following content: (1) mixes part basic asphalt, additive A and additive B; (2) in the mixture obtaining to step (1), add addition of C, react, transpiring moisture then heats up; (3) remaining basic asphalt is added in the mixture that step (2) obtains, mix, obtain modifying asphalt product.
9. according to preparation method claimed in claim 8, it is characterized in that: step (1) adds 20wt%～40wt% basic asphalt, the mixing time of step (1) is 10～90 minutes, and mixing temperature is 90～150 ℃.
10. according to preparation method claimed in claim 8, it is characterized in that: in step (2), temperature of reaction is 90～150 ℃, and the reaction times is 0.5～8 hour; And then heat up 30～90 ℃, moisture is evaporated in mixture without bubble.
11. according to preparation method claimed in claim 8, it is characterized in that: in step (3), mixing time is 20～180 minutes, and mixing temperature is 120～280 ℃.
12. according to preparation method claimed in claim 8, it is characterized in that: add one or more in glycerol, rosin or naphthenic acid in step (1) and/or step (2), its add-on accounts for 0.5%～5% of modifying asphalt quality.
13. according to preparation method claimed in claim 8, it is characterized in that: remaining basic asphalt is added in the mixture that step (2) obtains, with 20～120 minutes, stir and be warming up to 160～280 ℃, mix.
14. according to preparation method claimed in claim 8, it is characterized in that: addition of C adds in the mode of bases aqueous solution of inorganic matter or water miscible liquid, wherein the concentration of sodium hydroxide and potassium hydroxide aqueous solution is 20wt% ~ saturated solution, lithium hydroxide aqueous solution concentration is 10wt% ~ saturated solution, and calcium hydroxide is 20wt% ~ 30wt% water miscible liquid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629389A (en) * | 2015-02-02 | 2015-05-20 | 浙江大学 | Flame retardant modified asphalt, flame retardant asphalt concrete and preparation method thereof, and application of slaked lime as flame retardant |
| CN105733279A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Wide-range asphalt and preparation method thereof |
| CN109207182A (en) * | 2018-10-09 | 2019-01-15 | 中国石油化工股份有限公司 | A kind of method of deasphalted oil production road asphalt |
| CN110872446A (en) * | 2018-08-30 | 2020-03-10 | 中国石油化工股份有限公司 | Modified road asphalt and preparation method thereof |
| CN111485083A (en) * | 2019-01-25 | 2020-08-04 | 南京理工大学 | Preparation method of ultrahigh-strength nano heterogeneous low-carbon steel |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105733279A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Wide-range asphalt and preparation method thereof |
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| CN110872446A (en) * | 2018-08-30 | 2020-03-10 | 中国石油化工股份有限公司 | Modified road asphalt and preparation method thereof |
| CN110872446B (en) * | 2018-08-30 | 2021-11-09 | 中国石油化工股份有限公司 | Modified road asphalt and preparation method thereof |
| CN109207182A (en) * | 2018-10-09 | 2019-01-15 | 中国石油化工股份有限公司 | A kind of method of deasphalted oil production road asphalt |
| CN109207182B (en) * | 2018-10-09 | 2021-07-20 | 中国石油化工股份有限公司 | Method for producing road asphalt by deasphalted oil |
| CN111485083A (en) * | 2019-01-25 | 2020-08-04 | 南京理工大学 | Preparation method of ultrahigh-strength nano heterogeneous low-carbon steel |
| CN111485083B (en) * | 2019-01-25 | 2021-09-10 | 南京理工大学 | Preparation method of ultrahigh-strength nano heterogeneous low-carbon steel |
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| CN103804925B (en) | 2016-01-20 |
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