CN110872448A - Ultraviolet aging resistant waste rubber powder modified asphalt and preparation method thereof - Google Patents
Ultraviolet aging resistant waste rubber powder modified asphalt and preparation method thereof Download PDFInfo
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- CN110872448A CN110872448A CN201810998791.XA CN201810998791A CN110872448A CN 110872448 A CN110872448 A CN 110872448A CN 201810998791 A CN201810998791 A CN 201810998791A CN 110872448 A CN110872448 A CN 110872448A
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- 239000010426 asphalt Substances 0.000 title claims abstract description 145
- 229920001971 elastomer Polymers 0.000 title claims abstract description 101
- 239000000843 powder Substances 0.000 title claims abstract description 97
- 239000002699 waste material Substances 0.000 title claims abstract description 78
- 230000032683 aging Effects 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- 238000010008 shearing Methods 0.000 claims abstract description 21
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 16
- 239000004611 light stabiliser Substances 0.000 claims abstract description 14
- 150000001412 amines Chemical class 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000011282 treatment Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007853 buffer solution Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 125000004018 acid anhydride group Chemical group 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 9
- 150000008064 anhydrides Chemical class 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- 230000035515 penetration Effects 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007983 Tris buffer Substances 0.000 claims description 5
- 238000005698 Diels-Alder reaction Methods 0.000 claims description 4
- XITRBUPOXXBIJN-UHFFFAOYSA-N bis(2,2,6,6-tetramethylpiperidin-4-yl) decanedioate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)CCCCCCCCC(=O)OC1CC(C)(C)NC(C)(C)C1 XITRBUPOXXBIJN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011280 coal tar Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- UFLXKQBCEYNCDU-UHFFFAOYSA-N (2,2,6,6-tetramethylpiperidin-4-yl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CC(C)(C)NC(C)(C)C1 UFLXKQBCEYNCDU-UHFFFAOYSA-N 0.000 claims description 3
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- WVRNUXJQQFPNMN-VAWYXSNFSA-N 3-[(e)-dodec-1-enyl]oxolane-2,5-dione Chemical compound CCCCCCCCCC\C=C\C1CC(=O)OC1=O WVRNUXJQQFPNMN-VAWYXSNFSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- FMRHJJZUHUTGKE-UHFFFAOYSA-N Ethylhexyl salicylate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1O FMRHJJZUHUTGKE-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229960000796 barbital sodium Drugs 0.000 claims description 2
- FTOAOBMCPZCFFF-UHFFFAOYSA-N barbitone sodium Natural products CCC1(CC)C(=O)NC(=O)NC1=O FTOAOBMCPZCFFF-UHFFFAOYSA-N 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- 239000000872 buffer Substances 0.000 claims description 2
- UONLDZHKYCFZRW-UHFFFAOYSA-N n-[6-[formyl-(2,2,6,6-tetramethylpiperidin-4-yl)amino]hexyl]-n-(2,2,6,6-tetramethylpiperidin-4-yl)formamide Chemical compound C1C(C)(C)NC(C)(C)CC1N(C=O)CCCCCCN(C=O)C1CC(C)(C)NC(C)(C)C1 UONLDZHKYCFZRW-UHFFFAOYSA-N 0.000 claims description 2
- 239000003027 oil sand Substances 0.000 claims description 2
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 2
- 229920005652 polyisobutylene succinic anhydride Polymers 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- RGHFKWPGWBFQLN-UHFFFAOYSA-M sodium;5,5-diethylpyrimidin-3-ide-2,4,6-trione Chemical compound [Na+].CCC1(CC)C([O-])=NC(=O)NC1=O RGHFKWPGWBFQLN-UHFFFAOYSA-M 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- CUXYLFPMQMFGPL-UHFFFAOYSA-N (9Z,11E,13E)-9,11,13-Octadecatrienoic acid Natural products CCCCC=CC=CC=CCCCCCCCC(O)=O CUXYLFPMQMFGPL-UHFFFAOYSA-N 0.000 claims 1
- CUXYLFPMQMFGPL-SUTYWZMXSA-N all-trans-octadeca-9,11,13-trienoic acid Chemical compound CCCC\C=C\C=C\C=C\CCCCCCCC(O)=O CUXYLFPMQMFGPL-SUTYWZMXSA-N 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000002585 base Substances 0.000 description 28
- 239000002245 particle Substances 0.000 description 13
- 239000007822 coupling agent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229920001690 polydopamine Polymers 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 229960001701 chloroform Drugs 0.000 description 4
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000010920 waste tyre Substances 0.000 description 2
- 238000006845 Michael addition reaction Methods 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 239000002262 Schiff base Substances 0.000 description 1
- 150000004753 Schiff bases Chemical class 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- -1 o-phenolic hydroxyl Chemical group 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000004151 quinonyl group Chemical group 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses ultraviolet aging resistant waste rubber powder modified asphalt and a preparation method thereof. The ultraviolet aging resistant waste rubber powder modified asphalt comprises the following raw material components in parts by weight: 100 parts of matrix asphalt; 15-35 parts of waste rubber powder; 0.2-3 parts of dopamine hydrochloride; 1-6 parts of hindered amine light stabilizer. The method comprises the steps of firstly carrying out primary modification on waste rubber powder by using dopamine hydrochloride, then further modifying the waste rubber powder by using a hindered amine light stabilizer, and finally carrying out mixing shearing and other treatments on the modified waste rubber powder and melted matrix asphalt to obtain the ultraviolet aging resistant waste rubber powder modified asphalt. The ultraviolet aging resistant waste rubber powder modified asphalt can solve the problems of poor storage stability and ultraviolet aging resistance, and has the advantages of simple preparation process, long ultraviolet aging resistant time and the like.
Description
Technical Field
The invention relates to waste rubber powder modified asphalt and a preparation method thereof, in particular to ultraviolet aging resistant waste rubber powder modified asphalt and a preparation method thereof.
Background
According to statistics, China has become the first automobile consuming country in the world for seven consecutive years, and the consumption numbers of cars are 2460 ten thousand and 2800 ten thousand respectively in 2015 and 2016; the yield of the latest waste rubber tires in 2017 is 6.35 hundred million, and the rubber tires are difficult to degrade, have long period and pollute the environment, so that great pressure is brought to the society. The rubber powder particles obtained by crushing the waste tires at normal temperature or low temperature are used for producing rubber powder modified asphalt to pave highways and airport runways, so that the method becomes an effective way for effectively solving the problem of the direction of the waste tires, and becomes an ideal environment-friendly pavement material. However, the rubber powder modified asphalt also faces some problems at present, such as poor compatibility between rubber powder and asphalt, insufficient stability and easy segregation; when the asphalt and the colloidal particles are radiated by ultraviolet for a long time, a series of physical and chemical changes can occur, so that the asphalt and the colloidal particles are hardened and embrittled, the damage strain is reduced, the asphalt and the colloidal particles are easy to crack, the bonding force between the asphalt and the colloidal particles is reduced, the asphalt and the colloidal particles are peeled off, and the service performance of the pavement is seriously influenced. Especially in areas with strong ultraviolet rays, the service life of the asphalt pavement is greatly shortened.
CN1765998A discloses a waste rubber powder modified asphalt composition and a preparation method thereof. The method uses a coupling agent to modify the surface of rubber powder, and utilizes the alkoxy in the coupling agent to form chemical combination with inorganic filler, carbon black and the like in the rubber powder, so as to form an organic active molecular layer between organic matters and inorganic matters, thereby improving the dispersibility of the rubber powder in asphalt.
US5704971 discloses a process for preparing an asphalt modifier using a homogeneous rubber powder. The method comprises the steps of firstly oxidizing the surface of rubber powder by using hydrogen peroxide to enable the surface of the rubber powder to generate more carboxyl due to oxidation, adding the oxidized rubber powder into asphalt added with a small amount of compatilizer, and stirring and developing to obtain the rubber powder modified asphalt. However, the use of hydrogen peroxide alone cannot make the surface of the rubber powder generate active groups, and cannot improve the compatibility of the rubber powder and the asphalt.
CN103146207A discloses an anti-ultraviolet aging composite modified asphalt and a preparation method thereof. The composite modified asphalt adopts the waste rubber powder subjected to swelling pretreatment to modify the matrix asphalt, and although the ultraviolet aging resistance of the asphalt is improved to a certain extent, the storage stability of the modified asphalt needs to be further improved.
CN101434472A discloses a method for improving the ultraviolet aging resistance of modified asphalt. In order to improve the ultraviolet aging resistance of the asphalt, the method adds an additive into the asphalt, wherein the additive is CeO with the function of absorbing ultraviolet rays2Nano-materials or anti-UV absorber UV-531. The ultraviolet absorbent used in the method is easy to volatilize and other loss problems when being mixed at high temperature, and CeO2The compatibility of the nano material and the asphalt is very poor, segregation and delamination are easy to occur, the play of the ultraviolet resistance of the nano material is influenced, and the improvement of the ultraviolet resistance and the aging resistance of the asphalt mixture is limited.
The prior art does not well solve the comprehensive problems of poor storage stability of the waste rubber powder modified asphalt and easy ultraviolet aging of common asphalt pavements, and has the defects of high cost, complex process and excessive use of organic additives. The light stabilizer is easily subjected to biological migration and volatilization by simply adding the light stabilizer into the asphalt, so that the ultraviolet aging resistance of the asphalt pavement is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides ultraviolet aging resistant waste rubber powder modified asphalt and a preparation method thereof. The ultraviolet aging resistant waste rubber powder modified asphalt can solve the problems of poor storage stability and ultraviolet aging resistance, and has the advantages of simple preparation process, long ultraviolet aging resistant time and the like.
The invention provides ultraviolet aging resistant waste rubber powder modified asphalt which comprises the following raw materials in parts by weight:
100 parts of matrix asphalt;
15-35 parts of waste rubber powder; preferably 20-35 parts;
0.2-3 parts of dopamine hydrochloride, preferably 0.2-1.5 parts;
1-6 parts of hindered amine light stabilizer.
Among them, the base asphalt is preferably an acid-anhydrified pre-modified base asphalt.
The pre-modified base asphalt with the acid anhydride group is obtained by Diels-Alder reaction of a substance with the acid anhydride group and the base asphalt.
The substance with acid anhydride group is one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, eleostearic anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolyzed polymaleic anhydride, and preferably maleic anhydride.
The matrix asphalt is one or more of petroleum asphalt, coal tar asphalt, oil sand asphalt and natural asphalt. The petroleum asphalt can be one or more selected from straight-run asphalt, solvent deoiled asphalt, oxidized asphalt and semi-oxidized asphalt, and the straight-run asphalt can be atmospheric residue obtained by atmospheric distillation of crude oil and can also be vacuum residue obtained by vacuum distillation of crude oil. The 25 ℃ penetration degree of the matrix asphalt is 50-3001/10 mm, and the softening point is 28-60 ℃.
The waste rubber powder can be various commercially available waste rubber powders, and the particle size of the waste rubber powder is 50-200 meshes.
The dopamine hydrochloride is common commercial dopamine hydrochloride.
The hindered amine light stabilizer is one or more of Tinuvin744, Tinuvin770, ADK Stab LA87, LuchemHAR100 and Uvinul 5050H, Uvinul 4050H.
The invention also provides a preparation method of the ultraviolet aging resistant waste rubber powder modified asphalt, which comprises the following steps:
(1) adding the waste rubber powder into water, and stirring to fully wet the rubber powder;
(2) adding dopamine hydrochloride into the mixed material obtained in the step (1) under the stirring condition, stirring, adding a buffer solution to adjust the pH value, and continuing stirring;
(3) filtering and drying the mixture obtained in the step (2) to obtain primarily modified waste rubber powder;
(4) adding the primarily modified waste rubber powder obtained in the step (3) and a hindered amine light stabilizer into an organic solvent, reacting under a heating reflux condition, cooling, filtering, washing and drying to obtain further modified waste rubber powder;
(5) and (4) adding the further modified waste rubber powder obtained in the step (4) into the melted matrix asphalt, and shearing, mixing and developing the mixture to obtain the ultraviolet aging resistant waste rubber powder modified asphalt.
Adding the further modified waste rubber powder obtained in the step (4) into the melted base asphalt, heating the mixture by a program, stirring the mixture, reacting the mixture in an inert gas atmosphere, and vacuumizing the reacted mixture; and shearing, mixing and developing the mixture obtained after the vacuumizing treatment to obtain the ultraviolet aging resistant waste rubber powder modified asphalt. Wherein the melting temperature of the matrix asphalt is 100-120 ℃, the temperature programming rate is 0.5-1 ℃/min, and the inert gas is N2The reaction conditions of the reaction are as follows: the reaction pressure is 0.05-0.2 MPa, preferably 0.1-0.15 MPa, the reaction temperature is 120-145 ℃, preferably 125-140 ℃, and the reaction time is 1-3 h; the time of the vacuum pumping treatment is 10-60 min, preferably 10-45 min, and the vacuum degree is 0.02-0.09 MPa, preferably 0.02-0.07 MPa. The shearing temperature is 150-220 ℃, the optimal shearing temperature is 170-200 ℃, the shearing time is 30-200 min, the optimal shearing time is 50-180 min, and the shearing speed is 4000-7000 r/min.
Wherein the base asphalt in the step (5) is preferably anhydrifiedPre-modifying the base asphalt. The acid anhydrified pre-modified base asphalt can be prepared by the following method: adding the heated and melted matrix asphalt into a reactor, controlling the reaction temperature and pressure, and carrying out Diels-Alder reaction with the substance with the acid anhydride group in the inert gas atmosphere to obtain the pre-modified matrix asphalt with the acid anhydride group. The inert gas is N2The reaction time is 3-6 h, the reaction temperature is 120-160 ℃, and the reaction pressure is 0.2-0.7 MPa, preferably 0.25-0.5 MPa. The weight ratio of the substances with the acid anhydride groups to the matrix asphalt is (1-10): 100, preferably (2-6): 100.
in the step (1), the weight ratio of the waste rubber powder to the water is 1: (3-10). Wherein, the water can adopt deionized water.
In the step (2), the stirring conditions after adding the dopamine hydrochloride and before adding the buffer solution are as follows: the stirring time is preferably 20-40 min; adjusting the pH value to 8.0-9.0; the stirring conditions after adding the buffer were: the stirring temperature is 15-45 ℃, preferably 20-35 ℃, and the stirring time is 18-72 hours, preferably 24-48 hours.
In the step (2), the buffer solution is one or more of a tris buffer solution, a barbital sodium buffer solution, a borax buffer solution and a sodium hydroxide buffer solution, and is preferably a tris buffer solution.
In the step (3), the filtration and the drying can be carried out by the conventional technology. And drying to volatilize the surface moisture of the obtained primarily modified waste rubber powder, wherein the drying temperature is 60-80 ℃, and the drying time is 2-6 h.
In the step (4), the weight ratio of the preliminarily modified waste rubber powder to the organic solvent is 1: (10-30). The organic solvent is one or more of trichloromethane, carbon tetrachloride, acetone, ethanol, cyclohexane, benzene, toluene, xylene and cyclohexanone.
In the step (4), the reaction temperature is 50-90 ℃, preferably 60-90 ℃, and the reaction time is 6-8 hours. The filtration, washing and drying can be carried out by the conventional technology. The washing can be carried out by using solvents such as ethanol, chloroform, acetone and the like, and the drying is carried out to volatilize the solvents, wherein the drying temperature is 80-120 ℃, and the drying time is 3-8 h.
In the step (5), the melting temperature of the matrix asphalt is 100-120 ℃, the shearing temperature is 150-220 ℃, the shearing time is 30-200 min, the shearing time is 50-180 min, and the shearing speed is 4000-7000 r/min.
Compared with the prior art, the ultraviolet aging resistant waste rubber powder modified asphalt has the following advantages:
(1) the waste rubber powder particles are preliminarily modified by using the dopamine hydrochloride, the polydopamine can be tightly bonded with organic and inorganic fillers in the rubber powder at the same time, the stability is extremely high, and the polydopamine is not influenced in strong acid, strong alkali, ultrasonic oscillation and water environment. The rubber powder surface after preliminary modification contains a large amount of functional groups such as o-phenolic hydroxyl, carboxyl, amino, quinonyl and the like, so that a level-two reaction platform can be provided for the subsequent reaction with asphalt, the compatibility of the waste rubber powder and the asphalt is improved, and the segregation is prevented.
(2) The hindered amine light stabilizer and the active group on the dopamine hydrochloride are subjected to Michael addition reaction or Schiff base reaction, so that the hindered amine light stabilizer can be firmly fixed, and is prevented from physical migration and volatilization. The polydopamine and the hindered amine light stabilizer have better synergistic anti-aging effect after reacting.
(3) Under the condition of using a small amount of dopamine hydrochloride, the invention can increase the doping amount of the waste rubber powder, not only can improve the storage stability of the modified asphalt, but also can reduce the production cost of the waste rubber powder modified asphalt.
(4) The invention adopts the pre-modified base asphalt which is anhydrified, the pre-modified base asphalt has better cementation with the waste rubber particles after being modified by dopamine hydrochloride and hindered amine light stabilizer, and eliminates the adverse effect of hydrophilic groups on the surface of polydopamine on compatibility, thereby improving the storage stability and the ultraviolet aging resistance of the rubber powder modified asphalt without influencing other performances of the asphalt. Meanwhile, a large number of surface active groups of polydopamine can react with unreacted micromolecular anhydride, so that volatilization of micromolecules is prevented to a great extent, and harm to human bodies and the environment is reduced.
(5) The surface modification process of the waste rubber powder is completely carried out in the water phase, a large amount of organic solvent and other additives are not needed, the damage to human bodies and the environment is avoided, the modification process is simple, and the large-scale production and construction are convenient.
Detailed Description
The technical solution of the present invention is further described below by way of examples, but these examples are not intended to limit the present invention, and wt% referred to is mass fraction.
Example 1
(1) Adding 23 parts by weight of 60-mesh waste rubber powder into 120 parts by weight of deionized water, and quickly stirring to fully wet rubber powder particles.
(2) Slowly adding 0.4 part by weight of dopamine hydrochloride into the mixed material obtained in the step (1) under the condition of continuously stirring, continuously stirring for 30min, and adding a proper amount of tris buffer solution to adjust the pH value of the mixed solution to 8.0. The mixture was kept stirring for 24h in a thermostated water bath at 25 ℃.
(3) And (3) filtering the mixed material obtained in the step (2), and drying at 70 ℃ for 4h to obtain the primarily modified waste rubber powder.
(4) Adding the preliminarily modified waste rubber powder obtained in the step (3) and 2 parts by weight of Tinuvin770 into 400 parts by weight of ethanol. Keeping the temperature at 70 ℃, continuously stirring, heating and refluxing for 6h, cooling, filtering, washing with ethanol, and drying at 100 ℃ for 8h to obtain the further modified waste rubber powder.
(5) Adding the further modified waste rubber powder obtained in the step (4) into 100 parts of base asphalt which is heated and melted at 115 ℃ (the base asphalt is coal tar asphalt, the penetration degree (1/10mm) at 25 ℃ is 95, the softening point is 54 ℃), heating to 130 ℃ at the speed of 0.7 ℃/min, continuously stirring, stirring at 0.1MPa and N2Reacting for 2 hours under the atmosphere; the reaction-terminated mixture was evacuated under a vacuum of 0.02MPa for 20 min.
(6) And (3) continuously shearing the mixture obtained in the step (5) at the temperature of 170 ℃ at 5000r/min for 50min to uniformly disperse the mixture in the asphalt to obtain the ultraviolet aging resistant waste rubber powder modified asphalt A1.
Example 2
(1) Adding 30 parts by weight of 100-mesh waste rubber powder into 280 parts by weight of deionized water, and quickly stirring to fully wet rubber powder particles.
(2) Slowly adding 0.7 weight part of dopamine hydrochloride buffer solution into the mixed material obtained in the step (1) under the condition of continuously stirring, and after continuously stirring for 35min, adding a proper amount of tris (hydroxymethyl) aminomethane to adjust the pH value of the mixed solution to 8.5. The mixture was kept stirring for 30h in a 30 ℃ constant temperature water bath.
(3) And (3) filtering the mixed material obtained in the step (2), and drying at 75 ℃ for 6h to obtain the primarily modified waste rubber powder.
(4) Adding the preliminary modified waste rubber powder obtained in the step (3) and 3 parts by weight of ADK Stab LA87 into 350 parts by weight of chloroform. Keeping the temperature at 70 ℃, continuously stirring, heating and refluxing for 7h, cooling, filtering, washing with chloroform, and drying at 100 ℃ for 4h to obtain the further modified waste rubber powder particles.
(5) Adding the further modified waste rubber powder obtained in the step (4) into 100 parts of base asphalt which is heated and melted at 100 ℃ (the base asphalt is petroleum asphalt, the penetration degree (1/10mm) at 25 ℃ is 93, the softening point is 57 ℃), raising the temperature to 130 ℃ at the speed of 0.5 ℃/min, continuously stirring, stirring at 0.1MPa and N2Reacting for 2 hours under the atmosphere; the reaction-terminated mixture was evacuated under a vacuum of 0.03MPa for 40 min.
(6) And (3) continuously shearing the mixture obtained in the step (5) at the temperature of 180 ℃ at 4000r/min for 100min to uniformly disperse the mixture in the asphalt to obtain the ultraviolet aging resistant waste rubber powder modified asphalt A2.
Example 3
The other steps are the same as example 1, except that the base asphalt used in the step (5) is changed into the pre-modified base asphalt which is anhydrified, and finally the ultraviolet aging resistant waste rubber powder modified asphalt A3 is prepared.
Wherein the pre-modified base asphalt subjected to anhydrization is prepared by the following method: 100 parts of base asphalt (same as example 1) heated to 120 ℃ is added into a reactor, 4 parts of maleic anhydride is added, the temperature is raised to 130 ℃, and N is introduced after the pressure is stable2And keeping the total pressure at 0.25MPa, stirring and reacting for 4 hours at constant temperature and pressure, and slowly releasing the pressure to obtain the pre-modified base asphalt subjected to anhydrization.
Example 4
The other steps are the same as example 2, except that the base asphalt used in the step (5) is changed into the pre-modified base asphalt which is anhydrified, and finally the ultraviolet aging resistant waste rubber powder modified asphalt A4 is prepared.
Wherein the pre-modified base asphalt subjected to anhydrization is prepared by the following method: 100 parts of base asphalt (same as example 2) heated to 150 ℃ is added into a reactor, 3 parts of maleic anhydride is added, the temperature is raised to 140 ℃, and N is introduced after the pressure is stable2And keeping the total pressure at 0.35MPa, stirring and reacting for 3 hours at constant temperature and pressure, and slowly releasing the pressure to obtain the pre-modified base asphalt subjected to anhydrization.
Example 5
Step (1) to step (4) were the same as in example 1; and (3) adding the further modified waste rubber powder obtained in the step (4) into 100 parts of base asphalt which is heated and melted at the temperature of 115 ℃ (the base asphalt is coal tar asphalt, the penetration degree (1/10mm) at the temperature of 25 ℃ is 95, and the softening point is 54 ℃), and continuously shearing the mixture at the temperature of 170 ℃ at 5000r/min for 50min to uniformly disperse the mixture in asphalt, so that the ultraviolet aging resistant waste rubber powder modified asphalt A5 is obtained.
Comparative example 1
23 parts by weight of unmodified 60-mesh waste rubber powder and 2 parts by weight of Tinuvin770 were added to 100 parts of 115 ℃ heat-melted base asphalt (same as example 1), and the mixture was continuously sheared at 5000r/min at 170 ℃ for 50min to be uniformly dispersed in the asphalt, thereby obtaining comparative example waste rubber powder modified asphalt D1.
Comparative example 2
(1) Preparing coupling agent hydrolysate by using KH550 coupling agent, deionized water and alcohol (coupling agent: deionized water: alcohol =1:1: 20).
(2) Adding 20 parts by weight of 60-mesh waste rubber powder into 100 parts by weight of coupling agent hydrolysate, stirring for 30min, filtering the mixed solution, drying at 60 ℃ for 6h, and removing water on the surface of rubber powder to obtain coupling agent modified waste rubber powder particles.
(3) Waste rubber powder obtained in the step (2) after the coupling agent is modified and 1 part of nano CeO by weight2And 0.06 part by weight of an ultraviolet-resistant absorbent UV-531 (2-hydroxy-4-n-octyloxybenzophenone) were added to 100 parts of the base asphalt (same as in example 2) which was melted by heating, and the mixture was continuously sheared at 5000r/min at 170 ℃ for 50min to be uniformly dispersed in the asphalt, thereby obtaining a comparative example waste rubber powder-modified asphalt D2.
Test example
The ultraviolet aging test is carried out in an ultraviolet aging box, and the ultraviolet intensity is 1200 mu w/cm2The aging temperature is 60 ℃, and the aging time is 6 days. The test results are as follows:
TABLE 1 comparison of Properties of modified asphalts of examples and comparative examples after UV aging
| Modified asphalt | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
| Penetration ratio/%) | 61 | 65 | 70 | 73 | 58 | 56 | 58 |
| Increase in softening Point/. degree.C | 8 | 6 | 4 | 2.5 | 11 | 14 | 12 |
| Ductility per cm at 10 DEG C | 52 | 56 | 59 | 64 | 44 | 30 | 32 |
| Residual ductility ratio/10 ℃% | 58 | 62 | 65 | 77 | 50 | 39 | 42 |
| Storage stability/. degree.C. (163 ℃ C., 48h, isolation, poor softening point) | 2.2 | 2.4 | 1.6 | 2.0 | 2.6 | 6.5 | 4.1 |
Claims (17)
1. The ultraviolet aging resistant waste rubber powder modified asphalt comprises the following raw material components in parts by weight:
100 parts of matrix asphalt;
15-35 parts of waste rubber powder; preferably 20-35 parts;
0.2-3 parts of dopamine hydrochloride, preferably 0.2-1.5 parts;
1-6 parts of hindered amine light stabilizer.
2. The modified asphalt of claim 1, wherein: the base asphalt is pre-modified base asphalt which is anhydrized.
3. The modified asphalt according to claim 2, wherein: the pre-modified base asphalt with the acid anhydride group is obtained by Diels-Alder reaction of a substance with the acid anhydride group and the base asphalt.
4. The modified asphalt according to claim 3, wherein: the substance with acid anhydride group is one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, dodecenyl succinic anhydride, eleostearic acid anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolytic polymaleic anhydride, and preferably maleic anhydride.
5. The modified asphalt according to claim 1 or 2, characterized in that: the matrix asphalt is one or more of petroleum asphalt, coal tar asphalt, oil sand asphalt and natural asphalt; the 25 ℃ penetration degree of the matrix asphalt is 50-3001/10 mm, and the softening point is 28-60 ℃.
6. The modified asphalt of claim 1, wherein: the granularity of the waste rubber powder is 50-200 meshes.
7. The modified asphalt of claim 1, wherein: the hindered amine light stabilizer is one or more of Tinuvin744, Tinuvin770, ADK Stab LA87, Luchem HAR100 and Uvinul 5050H, Uvinul 4050H.
8. A method for preparing the ultraviolet aging resistant waste rubber powder modified asphalt as claimed in any one of claims 1 to 7, comprising the following steps:
(1) adding the waste rubber powder into water, and stirring to fully wet the rubber powder;
(2) adding dopamine hydrochloride into the mixed material obtained in the step (1) under the stirring condition, stirring, adding a buffer solution to adjust the pH value, and continuing stirring;
(3) filtering and drying the mixture obtained in the step (2) to obtain primarily modified waste rubber powder;
(4) adding the primarily modified waste rubber powder obtained in the step (3) and a hindered amine light stabilizer into an organic solvent, reacting under a heating reflux condition, cooling, filtering, washing and drying to obtain further modified waste rubber powder;
(5) and (4) adding the further modified waste rubber powder obtained in the step (4) into the melted matrix asphalt, and shearing, mixing and developing the mixture to obtain the ultraviolet aging resistant waste rubber powder modified asphalt.
9. The method of claim 8, wherein: step (5) adding the further modified waste rubber powder obtained in the step (4) into the melted matrix asphalt, heating the mixture by a program, stirring the mixture, reacting the mixture in an inert gas atmosphere, and vacuumizing the reacted mixture; and shearing, mixing and developing the mixture obtained after the vacuumizing treatment to obtain the ultraviolet aging resistant waste rubber powder modified asphalt.
10. The method of claim 9, wherein: in the step (5), the temperature programming rate is 0.5-1 ℃/min, and the inert gas is N2The reaction conditions of the reaction are as follows: the reaction pressure is 0.05-0.2 MPa, preferably 0.1-0.15 MPa, the reaction temperature is 120-145 ℃, preferably 125-140 ℃, and the reaction time is 1-3 h; the time of the vacuum pumping treatment is 10-60 min, preferably 10-45 min, and the vacuum degree is 0.02-0.09 MPa, preferably 0.02-0.07 MPa.
11. The method of claim 8, 9 or 10, wherein: the base asphalt in step (5) is preferably an acid anhydrified pre-modified base asphalt; the preparation method of the anhydrified pre-modified base asphalt comprises the following steps: adding the heated and melted matrix asphalt into a reactor, controlling the reaction temperature and pressure, and carrying out Diels-Alder reaction with the substance with the acid anhydride group in the inert gas atmosphere to obtain the pre-modified matrix asphalt with the acid anhydride group; wherein the weight ratio of the substance with the acid anhydride group to the matrix asphalt is (1-10): 100, preferably (2-6): 100, respectively; the inert gas being N2(ii) a The reaction time is 3-6 h, the reaction temperature is 120-160 ℃, and the reaction pressure is 0.2-0.7 MPa, preferably 0.25-0.5 MPa.
12. The method of claim 8, wherein: in the step (1), the weight ratio of the waste rubber powder to the water is 1: (3-10).
13. The method of claim 8, wherein: in the step (2), the stirring conditions after adding the dopamine hydrochloride and before adding the buffer solution are as follows: the stirring time is preferably 20-40 min; adjusting the pH value to 8.0-9.0; the stirring conditions after adding the buffer were: the stirring temperature is 15-45 ℃, preferably 20-35 ℃, and the stirring time is 18-72 hours, preferably 24-48 hours.
14. The method of claim 8, wherein: in the step (2), the buffer solution is one or more of a tris buffer solution, a barbital sodium buffer solution, a borax buffer solution and a sodium hydroxide buffer solution, and is preferably a tris buffer solution.
15. The method of claim 8, wherein: in the step (3), the drying temperature is 60-80 ℃ and the time is 2-6 h.
16. The method of claim 8, wherein: in the step (4), the organic solvent is one or more of chloroform, carbon tetrachloride, acetone, ethanol, cyclohexane, benzene, toluene, xylene and cyclohexanone; the weight ratio of the preliminarily modified waste rubber powder to the organic solvent is 1: (10-30); the reaction temperature is 50-90 ℃, preferably 60-90 ℃, and the reaction time is 6-8 h; the drying temperature is 80-120 ℃, and the drying time is 3-8 h.
17. The production method according to claim 8 or 9, characterized in that: in the step (5), the melting temperature of the matrix asphalt is 100-120 ℃, the shearing temperature is 150-220 ℃, the shearing time is 30-200 min, the shearing time is 50-180 min, and the shearing speed is 4000-7000 r/min.
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Effective date of registration: 20231013 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |