CN105037190A - Double-oil-chain and composite type slow-breaking quick-setting asphalt emulsifier as well as preparation method and application thereof - Google Patents
Double-oil-chain and composite type slow-breaking quick-setting asphalt emulsifier as well as preparation method and application thereof Download PDFInfo
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- 239000010426 asphalt Substances 0.000 title claims abstract description 92
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title abstract 2
- -1 polyoxyethylene Polymers 0.000 claims abstract description 13
- 229920000768 polyamine Polymers 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004698 Polyethylene Substances 0.000 claims description 9
- 229920000573 polyethylene Polymers 0.000 claims description 9
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 150000002632 lipids Chemical class 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical group NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- 229910015900 BF3 Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 abstract description 20
- 150000001768 cations Chemical class 0.000 abstract description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 3
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 125000003118 aryl group Chemical group 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 125000002091 cationic group Chemical group 0.000 description 14
- 238000000034 method Methods 0.000 description 14
- 238000010276 construction Methods 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 235000019738 Limestone Nutrition 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- 239000006028 limestone Substances 0.000 description 8
- 238000011056 performance test Methods 0.000 description 8
- 238000004945 emulsification Methods 0.000 description 6
- 238000012423 maintenance Methods 0.000 description 6
- 238000002329 infrared spectrum Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000008431 aliphatic amides Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a double-oil-chain and composite type slow-breaking quick-setting asphalt emulsifier as well as a preparation method and application thereof. The structural formula of the emulsifier is as follows (shown in the description), wherein m is equal to 10 or 15, r is equal to 3, 4 or 5, and n ranges from 12 to 18. According to the invention, by designing a novel double-oil-chain structure, the prepared emulsifier has an excellent emulsifying effect on asphalt of different types; by introducing the aromatic oleophylic chain, and using polyoxyethylene nonionic hydrophilic groups to replace partial polyamine cation hydrophilic groups, so that cation and nonionic compounding is realized, and an asphalt emulsion prepared from the emulsifier has an obvious slow-breaking property and is good in storage stability.
Description
Technical field
The present invention relates to a kind of preparation method and application of asphalt emulsifier, particularly relate to a kind of two oily chain, the compound preparation method and application splitting quick-setting asphalt emulsifying agent slowly.
Background technology
Along with the fast development of highway in China cause, the maintenance of road and maintenance problem are more and more subject to the attention of government and the people, and the important materials-pitch as maintenance road also causes the concern of people accordingly.Need to keep mobility in the use procedure of pitch, traditional heating method and solvent method all need mass energy, and can produce pollution; Emulsified bitumen is the advantage such as energy consumption is low, protection of the environment and be widely used in maintenance and the maintenance on road surface because having.The key raw material preparing emulsified bitumen is asphalt emulsifier, and asphalt emulsifier is divided into cationic, anionic, non-ionic type by ionic type.Compound asphalt emulsifier refers to and is carried out combining by the tensio-active agent of two or more type and the emulsifying agent having multiple advantage concurrently obtained, it can improve the performance of bitumen emulsion, larger meets the requirement of bitumen emulsion in construction, is therefore the asphalt emulsifier that a class has application prospect.Patent CN102604125A reports one and splits fast solidifying type asphalt emulsifier and its preparation method and application slowly, be composited by a certain percentage by Soxylat A 25-7, Trimethylamine 99 and epoxy chloropropane, this kind of emulsifier raw material is cheap, and obtained product is even, applied widely, shortcoming is that amount ratio is larger; Patent CN103709415A reports a kind of compound preparation method splitting slow hardening cation asphalt emulgent slowly, be composited by a certain percentage by hydroxylated vegetable oil, glycerol and phosphoric acid salt, the low price of this kind of emulsifying agent, synthesis technique is simple, and it is environmentally friendly, shortcoming is that cationic is weak, with building stones poor adhesion; Patent CN104387595A reports a kind of compound preparation method splitting slow hardening cation asphalt emulgent slowly, be composited by a certain percentage by xylogen, polyethylene polyamine, formaldehyde, Soxylat A 25-7, aliphatic amide etc., this emulsifier is few, the building stones be suitable for are wide, shortcoming is that synthetic route is long, complex process; Patent CN102924299A reports a kind of preparation method of novel slow-crack slow-coagulation asphalt emulsifier, be composited according to a certain percentage by long-chain fat amine, chloro fat alcohol and epoxy chloropropane, this kind of emulsifier ability is strong, good to the adhesivity of aggregate, bitumen emulsion uniform and smooth, stability in storage is good.Several emulsifying agents of above-mentioned report, oleophilic group structure is single, bad to the asphalt emulsification effect of different model.
This seminar devises a kind of novel two oily chain, compound asphalt emulsifier containing different structure, and because oleophilic group structure is different, it is all relatively good to the asphalt emulsification effect of multiple different model.The two oily chain structure of the compound asphalt emulsifier of present patent application, there is not yet reported in literature.
Summary of the invention
The object of this invention is to provide a kind of two oily chain, the compound preparation method splitting fast solidifying type asphalt emulsifier slowly.The present invention is by designing novel two oily chain structure, and obtained emulsifying agent all has good emulsifying effectiveness for the pitch of different model; Replace part polyamine cationic hydrophilic group by the oleophylic chain, the use polyoxyethylene non-ionic hydrophilic that introduce aromaticity, achieve positively charged ion and nonionic compound, make the slow fragility of bitumen emulsion with this emulsifying agent is obtained obvious, stability in storage is good.
The technical solution adopted in the present invention is:
A kind of two oily chain, compoundly split quick-setting asphalt emulsifying agent slowly, the structural formula of this emulsifying agent is as follows:
Wherein, m=10 or 15, r=3,4 or 5, n=12 ~ 18.
Described two oily chain, the compound preparation method splitting quick-setting asphalt emulsifying agent slowly, comprise the following steps:
1) Soxylat A 25-7 and catalyzer are joined in reactor, then drip epoxy chloropropane, in 60 ~ 80 DEG C of stirring reactions 10 ~ 18 hours, be cooled to room temperature, obtain intermediate a;
Wherein, mol ratio is epoxy chloropropane: Soxylat A 25-7=1 ~ 2:1, and catalyst quality is 0.1% ~ 0.3% of Soxylat A 25-7 and epoxy chloropropane quality sum;
2) polyethylene polyamine and intermediate a are mixed, be then warming up to 80 ~ 100 DEG C, and react 4 ~ 8 hours at this temperature, obtain intermediate b; Wherein, mol ratio is polyethylene polyamine: Soxylat A 25-7=0.8 ~ 1.2:1;
3) lipid acid is mixed with intermediate b, be then warming up to 130 ~ 160 DEG C, and react 3 ~ 7 hours at this temperature, obtain two oily chain, Compositional type asphalt emulsifier; Wherein, mol ratio is lipid acid: Soxylat A 25-7=1 ~ 1.8:1;
Described Soxylat A 25-7 is OP-10 or OP-15.
Described catalyzer is the vitriol oil, iron trichloride, aluminum chloride or boron trifluoride;
Described polyethylene polyamine is diethylenetriamine, triethylene tetramine or tetraethylene pentamine,
Described lipid acid is stearic acid, soy acid or appropriate that acid.
Described two oily chain, the compound application splitting quick-setting asphalt emulsifying agent slowly, comprise the following steps:
Prepared two oily chain, the compound quick-setting asphalt emulsifying agent that splits slowly are mixed with the aqueous solution that massfraction is 1 ~ 4%, after its pH value being transferred to 1 ~ 6 with hydrochloric acid again, be heated to 60 ~ 80 DEG C, stir in colloidal mill, add the heated bitumen of 120 ~ 150 DEG C, stir and namely obtain emulsified bitumen; Wherein asphalt content is 50% ~ 55% of emulsified bitumen total mass.
Innovative point of the present invention is the novelty in emulsifier molecules structure design and the popularity in the emulsifying agent scope of application.By designing the structure of two oily chain, can make containing long-chain, short-chain branch and fragrant chain in the lipophilic group of emulsifier molecules, the complicacy of oleophylic chain can make the pitch of emulsifier different model; Nonionogenic tenside and cats product compound use, make this emulsifying agent have the advantage of nonionogenic tenside and cats product: in mixed emulsifier, polyoxyethylene ether moiety provides slow fragility energy for bitumen emulsion simultaneously, after acidifying in cationic polyamines for bitumen emulsion provides better stability.
The present invention has following actively useful effect:
1, emulsifying agent of the present invention is because having the two oily chain structure of different structure, (as embodiment 1, embodiment 7, embodiment 8) emulsification can be carried out to Hebei interchannel pitch, Binzhou, Shandong pitch and Tianjin CNOOC pitch, the emulsion uniform and smooth obtained, all meet " highway asphalt construction technique normalizing " requirement, compared with general asphalt emulsifier, emulsifying agent of the present invention has the scope of application widely.
2, in Molecular Structure Design, not only embody positively charged ion and non-ionic feature, add the number of hydrophilic group simultaneously, significantly can reduce de-emulsification speed; Meanwhile, due to the mutual repulsion between cationic charge, improve the stability of emulsified bitumen.
3, (embodiment 1 and embodiment 2) the polyoxyethylene quantity in product of the present invention and polyethylene polyamine kind (embodiment 1 embodiment 5 and embodiment 6) adjustable, by regulating the quantity of oxyethyl group and the kind of polyethylene polyamine can adjust the HLB value of emulsifying agent and the sterically hindered of hydrophilic group, realizing the emulsification of dissimilar pitch and controlling de-emulsification speed and time of coagulation.
The stability in storage of the bitumen emulsion 4, obtained with product of the present invention all higher than 5 days of standard, and can reach 70 days.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained two oily chain, the compound infrared spectrum splitting quick-setting asphalt emulsifying agent slowly;
Fig. 2 is embodiment 1 gained two oily chain, the compound nuclear magnetic spectrogram splitting quick-setting asphalt emulsifying agent slowly.
Embodiment
Embodiment 1
The preparation of emulsifying agent: by 67.97g (0.1mol) OP-10 (polyoxyethylene nonylphenol ether-10), the 0.1mL vitriol oil (mass percent 95 ~ 98%) puts into there-necked flask, start to stir, the 80 DEG C of maintenances that heat up are constant, then 12.91g (0.14mol) epoxy chloropropane is slowly dripped, half an hour dropwises, and dropwises rear continuation reaction 12 hours, steams remaining epoxy chloropropane and namely obtains intermediate a;
18.90g (0.1mol) tetraethylene pentamine is joined in intermediate a, is warming up to 90 DEG C, stir 6 hours at this temperature, obtain intermediate b;
25.12g (0.1mol) soy acid is joined in intermediate b, is warming up to 150 DEG C, and stirring reaction 5 hours at this temperature, obtain two oily chain, compoundly split quick-setting asphalt emulsifying agent slowly.
This product sterling is carried out to the Preliminary detection of infrared spectra, as Fig. 1, find that there is the characteristic peak (broad peaks of more than 3600) of hydroxyl, the characteristic peak of the characteristic peak (about 3400) of amido and imido grpup and acid amides (absorption peak that primary amine 3424 place's stretching vibration is wide, carbonyl 1698 stretching vibration absorption peak and hydrogen bound to nitrogen 706 out-of-plane deformation vibration absorption peak).Meanwhile, carried out the detection of nuclear magnetic spectrogram to product, as Fig. 2, the peak major part appeared between 1 ~ 2 is the hydrogen in alkyl system for tax payment methylene; Peak major part between 3 ~ 4 is the hydrogen in Soxylat A 25-7 in methylene radical; About 7 peaks are benzene ring hydrogens; Peak between 2.3 ~ 3 is the hydrogen in the methylene radical in tetraethylene pentamine; The large peak at 2.17 places is the hydrogen in acetone impurity; The peak of some other reactive hydrogen all heterozygosis more than inside several peak.(as can be seen from nuclear magnetic spectrogram, total number of the hydrogen in spectrogram in total number of hydrogen and following structural formula matches; Although the number of the hydrogen of methylene radical and some difference of molecular formula of supposition in tetraethylene pentamine in nuclear-magnetism figure, but in conjunction with infrared spectrum, can find out that the peak (about 3400) of imino-again in infrared spectrum is very large, the structural unit by tetraethylene pentamine in molecule can be proved.Thus prove really to have synthesized the material with following structural formula.Wherein, m=10, r=4, n=16
The preparation of emulsifier aqueous solution: take this emulsifying agent of 2.0g, put into 100g water, emulsifier aqueous solution, to pH=4 ~ 5, is heated to 80 ~ 90 DEG C, can obtains emulsifier aqueous solution after emulsifiers dissolve by acid adjustment (using hydrochloric acid acid adjustment).
The preparation of bitumen emulsion: with the water preheat colloidal mill of 80 ~ 90 DEG C, the mentioned emulsifier aqueous solution is added in colloidal mill, then be that interchannel No. 70 heated bitumens of 120 ~ 130 DEG C add colloidal mill fast by 120g temperature, and constantly stir 1min, namely obtain even, fine and smooth bitumen emulsion.
The charge test of emulsified bitumen
The emulsified bitumen prepared is put into beaker.Be fixed on by two pieces of copper battery lead plates on a support, two electrode plate should parallel placement, then by stentplacement at content volume be 250mL beaker on.The emulsified bitumen sample prepared is poured among the beaker with battery lead plate, notice that pitch liquid level should higher than battery lead plate bottom, then battery lead plate wire being linked into respectively a volts DS is the both ends of power of 6V, after opening switch timing 5min, disconnecting power switch, observe the situation of positive pole and negative pole adsorptive pitch on battery lead plate, if the pitch on positive plate is more than on negative plate, and be adsorbed with a large amount of pitch particles, then prove that emulsified bitumen is anionic, otherwise negative plate is adsorbed with a large amount of pitch, then bitumen emulsion is cationic.
Other test experiments are all undertaken by " highway engineering pitch and asphalt Experimental Procedures " (People's Transportation Press, 2011 editions).
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 53.2%, and on sieve, residual content is 0.036%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 135min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 2
The preparation of emulsifying agent: change 67.97g (0.1mol) OP-10 into 83.60g (0.1mol) OP-15, all the other steps are with reference to embodiment 1.Obtain target emulsifying agent.Wherein, m=15, r=4, n=16
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: with the warm water preheating colloidal mill of 80 ~ 90 DEG C, the mentioned emulsifier aqueous solution is added in colloidal mill, then be that the heated bitumen of 120 ~ 130 DEG C adds colloidal mill fast by 100g temperature, and constantly stir 1min, namely obtain even, fine and smooth bitumen emulsion.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 53.5%, and on sieve, residual content is 0.052%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 140min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 3
The preparation of emulsifying agent: change 25.12g (0.1mol) soy acid into 26.18g (0.1mol) ready denier oil acid, all the other steps are with reference to embodiment 1.Obtain target emulsifying agent.Wherein, m=10, r=4, n=14
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 52.8%, and on sieve, residual content is 0.039%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 135min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 4
The preparation of emulsifying agent: change 25.12g (0.1mol) soy acid into 28.47g (0.1mol) stearic acid, all the other steps are with reference to embodiment 1.Obtain target emulsifying agent.Wherein, m=10, r=4, n=18
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 51.6%, and on sieve, residual content is 0.021%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 130min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 5
The preparation of emulsifying agent: change 18.90g (0.1mol) tetraethylene pentamine into 14.58g (0.1mol) triethylene tetramine, all the other steps are with reference to embodiment 1.Obtain target emulsifying agent.Wherein, m=10, r=3, n=16
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 53.8%, and on sieve, residual content is 0.131%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 130min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 6
The preparation of emulsifying agent: change 18.90g (0.1mol) tetraethylene pentamine into 10.31g (0.1mol) diethylenetriamine, all the other steps are with reference to embodiment 1.Obtain target emulsifying agent.Wherein, m=10, r=2, n=16
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 51.4%, and on sieve, residual content is 0.192%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 120min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 7
The preparation of emulsifying agent: repeat embodiment 1.
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: No. 90, the Shandong heated bitumen interchannel heated bitumen of 120 ~ 130 DEG C being changed into 120 DEG C ~ 130 DEG C, all the other steps repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 51.2%, and on sieve, residual content is 0.028%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 130min.Meet " highway asphalt construction technique normalizing " requirement.
Embodiment 8
The preparation of emulsifying agent: repeat embodiment 1.
The preparation of emulsifier aqueous solution: repeat embodiment 1.
The preparation of bitumen emulsion: CNOOC's No. 90 heated bitumens interchannel heated bitumen of 120 ~ 130 DEG C being changed into 110 DEG C ~ 120 DEG C, all the other steps repeat embodiment 1.
Through performance test data be: emulsified bitumen is cationic, can more than stable storage 5d, evaporation of residual amount is 50.6%, and on sieve, residual content is 0.019%, and be mixed into a grating limestone deposit material and split type slowly, the presetting period is 125min.Meet " highway asphalt construction technique normalizing " requirement.
Unaccomplished matter of the present invention is known technology.
Claims (6)
1. two oily chain, compoundly split a quick-setting asphalt emulsifying agent slowly, the structural formula that it is characterized by this emulsifying agent is as follows:
Wherein, m=10 or 15, r=3,4 or 5, n=12 ~ 18.
2. two oily chain, the compound preparation method splitting quick-setting asphalt emulsifying agent slowly as claimed in claim 1, is characterized by and comprise the following steps:
1) Soxylat A 25-7 and catalyzer are joined in reactor, then drip epoxy chloropropane, in 60 ~ 80 DEG C of stirring reactions 10 ~ 18 hours, be cooled to room temperature, obtain intermediate a;
Wherein, mol ratio is epoxy chloropropane: Soxylat A 25-7=1 ~ 2:1, and catalyst quality is 0.1% ~ 0.3% of Soxylat A 25-7 and epoxy chloropropane quality sum;
2) polyethylene polyamine and intermediate a are mixed, be then warming up to 80 ~ 100 DEG C, and react 4 ~ 8 hours at this temperature, obtain intermediate b; Wherein, mol ratio is polyethylene polyamine: Soxylat A 25-7=0.8 ~ 1.2:1;
3) lipid acid is mixed with intermediate b, be then warming up to 130 ~ 160 DEG C, and react 3 ~ 7 hours at this temperature, obtain two oily chain, Compositional type asphalt emulsifier; Wherein, mol ratio is lipid acid: Soxylat A 25-7=1 ~ 1.8:1;
Described catalyzer is the vitriol oil, iron trichloride, aluminum chloride or boron trifluoride.
3. two oily chain, the compound preparation method splitting quick-setting asphalt emulsifying agent slowly as claimed in claim 2, it is characterized by described Soxylat A 25-7 is OP-10 or OP-15.
4. two oily chain, the compound preparation method splitting quick-setting asphalt emulsifying agent slowly as claimed in claim 2, it is characterized by described polyethylene polyamine is diethylenetriamine, triethylene tetramine or tetraethylene pentamine.
5. two oily chain, the compound preparation method splitting quick-setting asphalt emulsifying agent slowly as claimed in claim 2, it is characterized by described lipid acid is stearic acid, soy acid or appropriate that acid.
6. two oily chain as claimed in claim 1, the compound application splitting quick-setting asphalt emulsifying agent slowly, is characterized by and comprise the following steps:
Two oily chain obtained above, the compound quick-setting asphalt emulsifying agent that splits slowly are mixed with the aqueous solution that massfraction is 1 ~ 4%, after its pH value being transferred to 1 ~ 6 with hydrochloric acid again, be heated to 60 ~ 80 DEG C, stir in colloidal mill, add the heated bitumen of 120 ~ 150 DEG C again, stir and namely obtain emulsified bitumen; Wherein asphalt content is 50% ~ 55% of emulsified bitumen total mass.
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