CN109355041A - A kind of asphalt modification water-proof emulsion and preparation method thereof - Google Patents
A kind of asphalt modification water-proof emulsion and preparation method thereof Download PDFInfo
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- CN109355041A CN109355041A CN201811245826.9A CN201811245826A CN109355041A CN 109355041 A CN109355041 A CN 109355041A CN 201811245826 A CN201811245826 A CN 201811245826A CN 109355041 A CN109355041 A CN 109355041A
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- 239000000839 emulsion Substances 0.000 title claims abstract description 80
- 239000010426 asphalt Substances 0.000 title claims abstract description 47
- 238000012986 modification Methods 0.000 title claims abstract description 41
- 230000004048 modification Effects 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000004945 emulsification Methods 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 229
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 108
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 31
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 26
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 25
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 13
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 103
- 239000000047 product Substances 0.000 claims description 90
- 238000002156 mixing Methods 0.000 claims description 81
- 238000012423 maintenance Methods 0.000 claims description 72
- 238000005406 washing Methods 0.000 claims description 68
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 58
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 28
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 14
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 11
- 238000003723 Smelting Methods 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 3
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000005292 vacuum distillation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 114
- 235000019441 ethanol Nutrition 0.000 description 36
- 239000000178 monomer Substances 0.000 description 9
- -1 2-ethyl hexyl acrylates Chemical class 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 8
- 229920001223 polyethylene glycol Polymers 0.000 description 8
- 239000002253 acid Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 3
- 241000255964 Pieridae Species 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 239000004908 Emulsion polymer Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 150000002240 furans Chemical class 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical group [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRXCDHOLJPJLLT-UHFFFAOYSA-N butane-2-sulfonic acid Chemical compound CCC(C)S(O)(=O)=O BRXCDHOLJPJLLT-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- CHDFNIZLAAFFPX-UHFFFAOYSA-N ethoxyethane;oxolane Chemical compound CCOCC.C1CCOC1 CHDFNIZLAAFFPX-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The present invention relates to a kind of asphalt modification water-proof emulsions and preparation method thereof.The asphalt modification water-proof emulsion is by 2- acrylamide-2-methyl propane sulfonic modified pitch, hydroxypropyl acrylate modified pitch, acrylate pre-emulsion and modified pitch composition, the 2- acrylamide-2-methyl propane sulfonic modified pitch is by pitch, toluene, dimethylbenzene, hydrogen peroxide, SE-10 emulsifier and the reaction of 2- acrylamide-2-methyl propane sulfonic are made, the hydroxypropyl acrylate modified pitch is by pitch, maleic anhydride, hydroxypropyl acrylate and toluene reaction are made, the acrylate pre-emulsion is by acrylic acid, butyl acrylate, Isooctyl acrylate monomer, 2-ethyl hexyl acrylate, 2- acrylamide-2-methyl propane sulfonic, the reactions such as AE-320 reactive emulsifier and ammonium persulfate are made, the modified pitch is made by reactions such as pitch and maleic anhydrides.Asphalt modification water-proof emulsion provided by the invention has excellent waterproof and tensile property.
Description
Technical field
The present invention relates to adhesive fields, and in particular to a kind of asphalt modification water-proof emulsion and preparation method thereof.
Background technique
With the rapid development of building decoration, client is higher and higher to the waterproof performance requirement of lotion, needs emulsion film forming
Water resistance reaches 48h or more afterwards, and the water resistance of existing lotion is only capable of reaching 15h, leads to existing high performance water proof lotion
It is monopolized by overseas enterprise, China needs to break the external monopoly position to water-proof emulsion field.Therefore, country encourages different necks
Domain research worker studies the material and method of water-proof emulsion.Since common water-proof emulsion is to there are waterproof performances and drawing
The defect of low strength is stretched, therefore, water-proof emulsion needs to improve in terms of waterproof and tensile property.
Summary of the invention
The purpose of the present invention is to provide a kind of asphalt modification water-proof emulsion, which uses 2- propylene
Amide -2- methyl propane sulfonic acid modified pitch, hydroxypropyl acrylate modified pitch, acrylate pre-emulsion and modified pitch are prepared into
It arrives, there is excellent waterproof and tensile property.
Another object of the present invention is to provide the preparation methods of above-mentioned asphalt modification water-proof emulsion.
To achieve the goals above, technical scheme is as follows:
A kind of asphalt modification water-proof emulsion is 5:7~16:68~83:3~8 2- acrylamide -2- by mass parts ratio
Methyl propane sulfonic acid modified pitch, hydroxypropyl acrylate modified pitch, acrylate pre-emulsion and modified pitch composition；Wherein, institute
The 2- acrylamide-2-methyl propane sulfonic modified pitch stated by mass parts ratio be 12:35~41:27~36:18~26:2~
Pitch, toluene, dimethylbenzene, hydrogen peroxide, SE-10 emulsifier and the 2- acrylamide-2-methyl propane sulfonic reaction system of 7:2~8
?；The hydroxypropyl acrylate modified pitch is 16:8~17:6~14:43~55 pitch, maleic by mass parts ratio
Dicarboxylic anhydride, hydroxypropyl acrylate and toluene reaction are made；The acrylate pre-emulsion is by mass parts ratio 4:16~23:14
~22:8~15:4~9:2~5:0.3~1:39~58:1~7 acrylic acid, butyl acrylate, Isooctyl acrylate monomer, propylene
Misery ester, 2- acrylamide-2-methyl propane sulfonic, AE-320 reactive emulsifier, ammonium persulfate, water and APE-2012 response type
Emulsifier reaction is made；The modified pitch is 10:9~15:4~12:6~11:0.3~1:60~65 by mass parts ratio
Pitch, maleic anhydride, polyethylene glycol 400, polytetrahydrofuran ether glycol PTMEG250, anhydrous aluminum chloride and dimethylbenzene it is anti-
It should be made.
Preferably, the 2- acrylamide-2-methyl propane sulfonic modified pitch, hydroxypropyl acrylate modified pitch, third
The mass parts ratio of olefin(e) acid ester pre-emulsion and modified pitch is 5:9.8:75:4.9.
The preparation method of above-mentioned asphalt modification water-proof emulsion, includes the following steps:
(1), pitch and maleic anhydride are added in mixer, 107~145 DEG C of conditions of maintenance system smelting temperature
15~50min of lower mixing, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and polyethylene glycol 400, poly- tetrahydro
Furans ether glycol PTMEG250, anhydrous aluminum chloride and toluene are added in reaction kettle, mixing speed 98r/min, reaction temperature
1~4h is reacted for 128~136 DEG C, -0.06MPa reduced-pressure backflow, product is evaporated under reduced pressure 1.5h, product through 143 DEG C, -0.09MPa
Through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；The polyethylene glycol 400 and poly- four
The purpose of hydrogen furans ether glycol PTMEG250 is to improve emulsion intercalation method；
(2), by acrylic acid, butyl acrylate, Isooctyl acrylate monomer, 2-ethyl hexyl acrylate, 2- acrylamide -2- methyl-prop sulphur
Acid, AE-320 reactive emulsifier, 1/4 ammonium persulfate of ammonium persulfate mass fraction total amount, water and APE-2012 response type
Emulsifier is added in reaction kettle, mixing speed 76r/min, reacts 0.5 under the conditions of 68~78 DEG C of maintenance system reaction temperature
Temperature of charge is cooled to 40 DEG C, remaining ammonium persulfate is added in reaction kettle by~2h, maintain under above-mentioned stirring condition after
Continuous reaction 35min, obtains acrylate pre-emulsion；The purpose of the 2- acrylamide-2-methyl propane sulfonic is to improve cream
The stability of liquid；
(3), pitch, maleic anhydride and toluene are added in reaction kettle, mixing speed 100r/min, maintain body
Be reaction temperature be 129~145 DEG C of 0.5~2h of reaction, product through 55 DEG C of 650mL water washing 4 times, 500mL ethanol washing 2 times,
It is dry, product and hydroxypropyl acrylate are added in reaction kettle, mixing speed 120r/min, maintenance system reaction temperature is
117~128 DEG C, -0.05MPa react 1.5~5h, product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry, i.e.,
Obtain hydroxypropyl acrylate modified pitch；The purpose of the hydroxypropyl acrylate is the chemical activity and stabilization to improve pitch
Property；
(4), pitch, toluene, dimethylbenzene, hydrogen peroxide and SE-10 emulsifier are added in hydrothermal reaction kettle, maintain water
Thermal response temperature is 49~63 DEG C of 13~41min of hydro-thermal reaction, product is transferred in reaction kettle, mixing speed 150r/
Min, 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, 2- acrylamide-2-methyl propane sulfonic are added to reaction
Kettle, mixing speed 115r/min, maintenance system reaction temperature is 119~132 DEG C, -0.07MPa reduced-pressure backflow reacts 2~6h,
Product is evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, product through 800mL water washing 3 times, 350mL ethanol washing 2 times, dry,
Obtain 2- acrylamide-2-methyl propane sulfonic modified pitch；The purpose of the 2- acrylamide-2-methyl propane sulfonic be for
Improve the chemical activity and stability of pitch；
(5), acrylate pre-emulsion and modified pitch are added in reaction kettle, mixing speed 110r/min, are maintained
25min is reacted under the conditions of 30 DEG C of system temperature, 2- acrylamide-2-methyl propane sulfonic modified pitch and hydroxypropyl acrylate are changed
The mixed liquor of property pitch is added in reaction kettle with 0.2 mass parts/min adding rate, maintains to continue under above-mentioned reaction condition
40min is reacted, temperature of reaction kettle is warming up to 72~86 DEG C of 1.5~5h of reaction, temperature of reaction kettle is cooled to 50 DEG C, in maintenance
The 20min that states under the conditions of mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
The beneficial effects of the present invention are:
1, pitch has excellent waterproofness, and polyethylene glycol 400 and polytetrahydrofuran ether glycol PTMEG250 are grafted to
Asphalt surface can improve the hydrophilic and oleophilic performance of pitch, improve the stability to oil hydrosol；The modified pitch of preparation is because having
Preferable hydrophilic and oleophilic performance can be obviously improved the stability, waterproofness and tensile property of water-proof emulsion；
2, while 2- acrylamide-2-methyl propane sulfonic and its polymer have higher chemical activity, have preferable
Emulsifiability can act synergistically with AE-320 reactive emulsifier and APE-2012 reactive emulsifier, improve anti-water and milk jointly
The stability of liquid；The substep addition of ammonium persulfate can effectively control the polymerization of monomer and 2- acrylamide-2-methyl propane sulfonic
Molecular weight improves emulsification and stability of the 2- acrylamide-2-methyl propane sulfonic prepolymer to lotion；The acrylate of preparation
Stability and tensile property of the pre-emulsion because being obviously improved water-proof emulsion with excellent stable emulsifying performance；
3 pitches have excellent waterproof performance, and hydroxypropyl acrylate is grafted to asphalt surface, improves the change of asphalt surface
Activity is learned, pitch is dispersed in water-proof emulsion polymer by way of chemical bond, the chemistry of water-proof emulsion can be obviously improved
Activity and waterproof performance；
4, pitch has excellent waterproof performance, and 2- acrylamide-2-methyl propane sulfonic is grafted to asphalt surface, improves
Pitch is dispersed in water-proof emulsion polymer by the chemical activity of asphalt surface by way of chemical bond, can improve anti-water and milk
The waterproof performance of liquid；
5, in 2- acrylamide-2-methyl propane sulfonic modified pitch, hydroxypropyl acrylate modified pitch, the pre- cream of acrylate
Under liquid and modified pitch synergistic effect, assign asphalt modification water-proof emulsion excellent stability, waterproofness and tensile property.
Specific embodiment
A specific embodiment of the invention is described below with reference to embodiment, to better understand the present invention.This
It is a little that examples are only for illustrating the present invention and not for limiting the scope of the present invention.Actual conditions are not specified in lower example embodiment
Experimental method, usually according to this field normal condition or the condition suggested according to manufacturer；Used raw material, reagent etc.,
It unless otherwise specified, is the raw materials and reagents that can be obtained from commercial sources such as conventional markets.Those skilled in the art is at this
The variation and replacement of any unsubstantiality done on the basis of invention belong to scope of the present invention.
Embodiment 1
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 11.9 parts of maleic anhydrides are added in mixer, maintenance system smelting temperature 123
Mixing 27min under the conditions of DEG C, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and 7.6 parts of polyethylene glycol
400,7.9 parts of polytetrahydrofuran ether glycol PTMEG250,0.4 part of anhydrous aluminum chloride and 63 parts of toluene are added in reaction kettle, are stirred
Mixing speed is 98r/min, and reaction temperature is 130 DEG C, -0.06MPa reduced-pressure backflow reacts 2.5h, and product is through 143 DEG C, -0.09MPa
Be evaporated under reduced pressure 1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 18.8 parts of butyl acrylates, 17.9 parts of Isooctyl acrylate monomers, 11.2 parts of 2-ethyl hexyl acrylates,
4.6 parts of 2- acrylamide-2-methyl propane sulfonics, 2.7 parts of AE-320 reactive emulsifiers, 0.1 part of ammonium persulfate, 43 parts of water and
2.1 parts of APE-2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, maintenance system reaction temperature 73
1h is reacted under the conditions of DEG C, temperature of charge is cooled to 40 DEG C, 0.3 part of ammonium persulfate is added in reaction kettle, is remained above-mentioned and is stirred
The reaction was continued under the conditions of mixing 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 11.3 parts of maleic anhydrides and 50 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 136 DEG C of reaction 1h, and product is washed through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 11.7 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, body is maintained
Be reaction temperature be 126 DEG C, -0.05MPa reacts 3.5h, product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry
It is dry to get arrive hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 38 parts of toluene, 31 parts of dimethylbenzene, 21 parts of hydrogen peroxide and 4.3 parts of SE-10 emulsifiers are added
Into hydrothermal reaction kettle, maintenance hydrothermal temperature is 55 DEG C of hydro-thermal reaction 27min, and product is transferred in reaction kettle, is stirred
Speed is 150r/min, 123 DEG C of maintenance system temperature, -0.06MPaIt is evaporated under reduced pressure 1h, by 3.4 parts of 2- acrylamide -2- methyl
Propane sulfonic acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 128 DEG C, -0.07MPa is depressurized back
Stream reaction 4h, product are evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, and product is through 800mL water washing 3 times, 350mL ethanol washing 2
It is secondary, dry to get arriving 2- acrylamide-2-methyl propane sulfonic modified pitch；
(5), 75 parts of acrylate pre-emulsions and 4.9 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 9.8
The mixed liquor of part hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, remains above-mentioned anti-
The reaction was continued under the conditions of answering 40min, is warming up to 78 DEG C of reaction 3h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50 DEG C, dimension
The 20min that holds under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 2
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 9 parts of maleic anhydrides are added in mixer, 107 DEG C of items of maintenance system smelting temperature
Mixing 50min under part, product is dry through 50 DEG C of 500mL water supersound washing 3 times, by product and 4 parts of polyethylene glycol 400s, 6 parts it is poly-
Tetrahydrofuran ether glycol PTMEG250,0.3 part of anhydrous aluminum chloride and 60 parts of toluene are added in reaction kettle, mixing speed 98r/
Min, reaction temperature is 128 DEG C, -0.06MPa reduced-pressure backflow reacts 4h, and product is evaporated under reduced pressure 1.5h through 143 DEG C, -0.09MPa,
Product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 16 parts of butyl acrylates, 14 parts of Isooctyl acrylate monomers, 8 parts of 2-ethyl hexyl acrylates, 4 parts of 2- third
Acrylamide -2- methyl propane sulfonic acid, 2 parts of AE-320 reactive emulsifiers, 0.075 part of ammonium persulfate, 39 parts of water and 1 part of APE-2012
Reactive emulsifier is added in reaction kettle, mixing speed 76r/min, is reacted under the conditions of 68 DEG C of maintenance system reaction temperature
Temperature of charge is cooled to 40 DEG C by 2h, and 0.225 part of ammonium persulfate is added in reaction kettle, maintain under above-mentioned stirring condition after
Continuous reaction 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 8 parts of maleic anhydrides and 43 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 129 DEG C of reaction 2h, and product is washed through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 6 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, maintenance system
Reaction temperature is 117 DEG C, -0.05MPa reacts 5h, and product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry, i.e.,
Obtain hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 35 parts of toluene, 27 parts of dimethylbenzene, 18 parts of hydrogen peroxide and 2 parts of SE-10 emulsifiers are added to
In hydrothermal reaction kettle, maintenance hydrothermal temperature is 49 DEG C of hydro-thermal reaction 41min, and product is transferred in reaction kettle, stirring speed
Degree is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 2 parts of 2- acrylamide -2- methyl-prop sulphurs
Acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 119 DEG C, -0.07MPa reduced-pressure backflow is anti-
Answer 6h, product is evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, product through 800mL water washing 3 times, 350mL ethanol washing 2 times,
It dries to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 68 parts of acrylate pre-emulsions and 3 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 7 parts
The mixed liquor of hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, maintains above-mentioned reaction
Under the conditions of the reaction was continued 40min, temperature of reaction kettle is warming up to 72 DEG C of reaction 5h, temperature of reaction kettle is cooled to 50 DEG C, is maintained
The reaction was continued under the conditions of above-mentioned mixing speed 20min is to get arriving asphalt modification water-proof emulsion.
Embodiment 3
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 15 parts of maleic anhydrides are added in mixer, 145 DEG C of maintenance system smelting temperature
Under the conditions of mixing 15min, product is dry through 50 DEG C of 500mL water supersound washing 3 times, by product and 12 parts of polyethylene glycol 400s, 11
Part polytetrahydrofuran ether glycol PTMEG250,1 part of anhydrous aluminum chloride and 65 parts of toluene are added in reaction kettle, and mixing speed is
98r/min, reaction temperature is 136 DEG C, -0.06MPa reduced-pressure backflow reacts 1h, and product is evaporated under reduced pressure through 143 DEG C, -0.09MPa
1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 23 parts of butyl acrylates, 22 parts of Isooctyl acrylate monomers, 15 parts of 2-ethyl hexyl acrylates, 9 parts of 2-
Acrylamide-2-methyl propane sulfonic, 5 parts of AE-320 reactive emulsifiers, 0.25 part of ammonium persulfate, 58 parts of water and 7 parts of APE-
2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, anti-under the conditions of 78 DEG C of maintenance system reaction temperature
0.5h is answered, temperature of charge is cooled to 40 DEG C, 0.75 part of ammonium persulfate is added in reaction kettle, is maintained under above-mentioned stirring condition
The reaction was continued 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 17 parts of maleic anhydrides and 55 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 145 DEG C of reaction 0.5h, and product is through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 14 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, body is maintained
Be reaction temperature be 128 DEG C, -0.05MPa reacts 1.5h, product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry
It is dry to get arrive hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 41 parts of toluene, 36 parts of dimethylbenzene, 26 parts of hydrogen peroxide and 7 parts of SE-10 emulsifiers are added to
In hydrothermal reaction kettle, maintenance hydrothermal temperature is 63 DEG C of hydro-thermal reaction 13min, and product is transferred in reaction kettle, stirring speed
Degree is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 8 parts of 2- acrylamide -2- methyl-prop sulphurs
Acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 132 DEG C, -0.07MPa reduced-pressure backflow is anti-
Answer 2h, product is evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, product through 800mL water washing 3 times, 350mL ethanol washing 2 times,
It dries to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 83 parts of acrylate pre-emulsions and 8 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 16
The mixed liquor of part hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, remains above-mentioned anti-
The reaction was continued under the conditions of answering 40min, is warming up to 86 DEG C of reaction 1.5h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50 DEG C,
The 20min that maintains under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 4
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 9.3 parts of maleic anhydrides are added in mixer, 109 DEG C of maintenance system smelting temperature
Under the conditions of mixing 17min, product is dry through 50 DEG C of 500mL water supersound washing 3 times, by product and 4.5 parts of polyethylene glycol 400s,
6.3 parts of polytetrahydrofuran ether glycol PTMEG250,0.4 part of anhydrous aluminum chloride and 61 parts of toluene are added in reaction kettle, stirring speed
Degree is 98r/min, and reaction temperature is 129 DEG C, -0.06MPa reduced-pressure backflow reacts 1.5h, and product is depressurized through 143 DEG C, -0.09MPa
Distill 1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 16.9 parts of butyl acrylates, 14.9 parts of Isooctyl acrylate monomers, 8.3 parts of 2-ethyl hexyl acrylates,
4.6 parts of 2- acrylamide-2-methyl propane sulfonics, 2.2 parts of AE-320 reactive emulsifiers, 0.09 part of ammonium persulfate, 40 parts of water and
1.3 parts of APE-2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, maintenance system reaction temperature 69
0.7h is reacted under the conditions of DEG C, temperature of charge is cooled to 40 DEG C, 0.27 part of ammonium persulfate is added in reaction kettle, is maintained above-mentioned
The reaction was continued under stirring condition 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 8.6 parts of maleic anhydrides and 45 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 130 DEG C of reaction 0.6h, and product is through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 6.7 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, is maintained
System reaction temperature is 118 DEG C, -0.05MPa reacts 1.8h, and product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry
It is dry to get arrive hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 36 parts of toluene, 28 parts of dimethylbenzene, 18.8 parts of hydrogen peroxide and 2.5 parts of SE-10 emulsifiers are added
Enter into hydrothermal reaction kettle, maintenance hydrothermal temperature is 50 DEG C of hydro-thermal reaction 14min, and product is transferred in reaction kettle, is stirred
Mixing speed is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 2.6 parts of 2- acrylamide -2- first
Base propane sulfonic acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 120 DEG C, -0.07MPa is depressurized
Back flow reaction 2.5h, product are evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, and product is through 800mL water washing 3 times, 350mL ethyl alcohol
It washs 2 times, dry to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 69 parts of acrylate pre-emulsions and 3.5 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 7.6
The mixed liquor of part hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, remains above-mentioned anti-
The reaction was continued under the conditions of answering 40min, is warming up to 73 DEG C of reaction 1.7h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50 DEG C,
The 20min that maintains under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 5
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 10.9 parts of maleic anhydrides are added in mixer, maintenance system smelting temperature 116
Mixing 21min under the conditions of DEG C, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and 6.5 parts of polyethylene glycol
400,8.6 parts of polytetrahydrofuran ether glycol PTMEG250,0.5 part of anhydrous aluminum chloride and 62 parts of toluene are added in reaction kettle, are stirred
Mixing speed is 98r/min, and reaction temperature is 130 DEG C, -0.06MPa reduced-pressure backflow reacts 2h, and product subtracts through 143 DEG C, -0.09MPa
Pressure distillation 1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 17.9 parts of butyl acrylates, 16.2 parts of Isooctyl acrylate monomers, 9.9 parts of 2-ethyl hexyl acrylates,
6.2 parts of 2- acrylamide-2-methyl propane sulfonics, 3.1 parts of AE-320 reactive emulsifiers, 0.12 part of ammonium persulfate, 41 parts of water and
2.8 parts of APE-2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, maintenance system reaction temperature 70
0.9h is reacted under the conditions of DEG C, temperature of charge is cooled to 40 DEG C, 0.36 part of ammonium persulfate is added in reaction kettle, is maintained above-mentioned
The reaction was continued under stirring condition 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 10.2 parts of maleic anhydrides and 46 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 132 DEG C of reaction 0.7h, and product is through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 8.8 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, is maintained
System reaction temperature is 120 DEG C, -0.05MPa reacts 1.9h, and product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry
It is dry to get arrive hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 38 parts of toluene, 29 parts of dimethylbenzene, 20.1 parts of hydrogen peroxide and 3.7 parts of SE-10 emulsifiers are added
Enter into hydrothermal reaction kettle, maintenance hydrothermal temperature is 53 DEG C of hydro-thermal reaction 17min, and product is transferred in reaction kettle, is stirred
Mixing speed is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 3.6 parts of 2- acrylamide -2- first
Base propane sulfonic acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 123 DEG C, -0.07MPa is depressurized
Back flow reaction 3.5h, product are evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, and product is through 800mL water washing 3 times, 350mL ethyl alcohol
It washs 2 times, dry to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 75 parts of acrylate pre-emulsions and 4.5 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 9.8
The mixed liquor of part hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, remains above-mentioned anti-
The reaction was continued under the conditions of answering 40min, is warming up to 77 DEG C of reaction 3h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50 DEG C, dimension
The 20min that holds under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 6
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 10 parts of maleic anhydrides are added in mixer, 125 DEG C of maintenance system smelting temperature
Under the conditions of mixing 30min, product is dry through 50 DEG C of 500mL water supersound washing 3 times, by product and 8 parts of polyethylene glycol 400s, 9 parts
Polytetrahydrofuran ether glycol PTMEG250,0.7 part of anhydrous aluminum chloride and 64 parts of toluene are added in reaction kettle, and mixing speed is
98r/min, reaction temperature is 132 DEG C, -0.06MPa reduced-pressure backflow reacts 3h, and product is evaporated under reduced pressure through 143 DEG C, -0.09MPa
1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 19 parts of butyl acrylates, 17 parts of Isooctyl acrylate monomers, 11 parts of 2-ethyl hexyl acrylates, 6 parts of 2-
Acrylamide-2-methyl propane sulfonic, 3 parts of AE-320 reactive emulsifiers, 0.15 part of ammonium persulfate, 45 parts of water and 6 parts of APE-
2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, anti-under the conditions of 75 DEG C of maintenance system reaction temperature
Answer 1h, temperature of charge be cooled to 40 DEG C, 0.45 part of ammonium persulfate is added in reaction kettle, maintain under above-mentioned stirring condition after
Continuous reaction 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 14 parts of maleic anhydrides and 50 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 140 DEG C of reaction 1h, and product is washed through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 12 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, maintenance system
Reaction temperature is 123 DEG C, -0.05MPa reacts 3h, and product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry, i.e.,
Obtain hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 40 parts of toluene, 30 parts of dimethylbenzene, 22 parts of hydrogen peroxide and 5 parts of SE-10 emulsifiers are added to
In hydrothermal reaction kettle, maintenance hydrothermal temperature is 55 DEG C of hydro-thermal reaction 30min, and product is transferred in reaction kettle, stirring speed
Degree is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 6 parts of 2- acrylamide -2- methyl-prop sulphurs
Acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 125 DEG C, -0.07MPa reduced-pressure backflow is anti-
Answer 3h, product is evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, product through 800mL water washing 3 times, 350mL ethanol washing 2 times,
It dries to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 76 parts of acrylate pre-emulsions and 5 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and 13
The mixed liquor of part hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, remains above-mentioned anti-
The reaction was continued under the conditions of answering 40min, is warming up to 80 DEG C of reaction 3h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50 DEG C, dimension
The 20min that holds under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 7
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 14.6 parts of maleic anhydrides are added in mixer, maintenance system smelting temperature 143
Mixing 45min under the conditions of DEG C, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and 11.3 parts of polyethylene glycol
400,10.5 parts of polytetrahydrofuran ether glycol PTMEG250,0.9 part of anhydrous aluminum chloride and 64 parts of toluene are added in reaction kettle, are stirred
Mixing speed is 98r/min, and reaction temperature is 135 DEG C, -0.06MPa reduced-pressure backflow reacts 3.5h, and product is through 143 DEG C, -0.09MPa
Be evaporated under reduced pressure 1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 22.6 parts of butyl acrylates, 21.7 parts of Isooctyl acrylate monomers, 14.6 parts of 2-ethyl hexyl acrylates,
8.6 parts of 2- acrylamide-2-methyl propane sulfonics, 4.6 parts of AE-320 reactive emulsifiers, 0.24 part of ammonium persulfate, 55 parts of water and
6.5 parts of APE-2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, maintenance system reaction temperature 75
1.8h is reacted under the conditions of DEG C, temperature of charge is cooled to 40 DEG C, 0.72 part of ammonium persulfate is added in reaction kettle, is maintained above-mentioned
The reaction was continued under stirring condition 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 15.8 parts of maleic anhydrides and 53.2 parts of toluene are added in reaction kettle, mixing speed
For 100r/min, maintenance system reaction temperature is 144 DEG C of reaction 1.8h, and product is through 55 DEG C of 650mL water washing 4 times, 500mL second
Alcohol washs 2 times, drying, product and 13.2 parts of hydroxypropyl acrylates is added in reaction kettle, mixing speed 120r/min, ties up
Hold that system reaction temperature is 126 DEG C, -0.05MPa reacts 4.5h, product through 750mL water washing 3 times, 300mL ethanol washing 2 times,
It dries to get hydroxypropyl acrylate modified pitch is arrived；
(4), 12 parts of pitches, 40 parts of toluene, 35 parts of dimethylbenzene, 25 parts of hydrogen peroxide and 6.5 parts of SE-10 emulsifiers are added
Into hydrothermal reaction kettle, maintenance hydrothermal temperature is 62 DEG C of hydro-thermal reaction 40min, and product is transferred in reaction kettle, is stirred
Speed is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 7.5 parts of 2- acrylamide -2- methyl
Propane sulfonic acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 131 DEG C, -0.07MPa is depressurized back
Stream reaction 5.5h, product are evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, and product is washed through 800mL water washing 3 times, 350mL ethyl alcohol
It washs 2 times, dry to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 81 parts of acrylate pre-emulsions and 7.1 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and
The mixed liquor of 15.5 parts of hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, in maintenance
The 40min that states under reaction condition that the reaction was continued, is warming up to 82 DEG C of reaction 4.3h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50
DEG C, the 20min that maintains under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Embodiment 8
A kind of asphalt modification water-proof emulsion, preparation method includes the following steps:
(1), 10 parts of pitches and 13.1 parts of maleic anhydrides are added in mixer, maintenance system smelting temperature 132
Mixing 36min under the conditions of DEG C, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and 10.8 parts of polyethylene glycol
400,8.9 parts of polytetrahydrofuran ether glycol PTMEG250,0.8 part of anhydrous aluminum chloride and 63 parts of toluene are added in reaction kettle, are stirred
Mixing speed is 98r/min, and reaction temperature is 132 DEG C, -0.06MPa reduced-pressure backflow reacts 2.8h, and product is through 143 DEG C, -0.09MPa
Be evaporated under reduced pressure 1.5h, product through 500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by 4 parts of acrylic acid, 20.7 parts of butyl acrylates, 19.2 parts of Isooctyl acrylate monomers, 13.3 parts of 2-ethyl hexyl acrylates,
7.3 parts of 2- acrylamide-2-methyl propane sulfonics, 3.9 parts of AE-320 reactive emulsifiers, 0.17 part of ammonium persulfate, 45 parts of water and
4.5 parts of APE-2012 reactive emulsifiers are added in reaction kettle, mixing speed 76r/min, maintenance system reaction temperature 73
1.7h is reacted under the conditions of DEG C, temperature of charge is cooled to 40 DEG C, 0.51 part of ammonium persulfate is added in reaction kettle, is maintained above-mentioned
The reaction was continued under stirring condition 35min, obtains acrylate pre-emulsion；
(3), 16 parts of pitches, 14.1 parts of maleic anhydrides and 46 parts of toluene are added in reaction kettle, mixing speed is
100r/min, maintenance system reaction temperature are 141 DEG C of reaction 1.8h, and product is through 55 DEG C of 650mL water washing 4 times, 500mL ethyl alcohol
2 times, drying are washed, product and 12.2 parts of hydroxypropyl acrylates are added in reaction kettle, mixing speed 120r/min, is maintained
System reaction temperature is 121 DEG C, -0.05MPa reacts 3.7h, and product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry
It is dry to get arrive hydroxypropyl acrylate modified pitch；
(4), 12 parts of pitches, 39 parts of toluene, 32 parts of dimethylbenzene, 23 parts of hydrogen peroxide and 5.2 parts of SE-10 emulsifiers are added
Into hydrothermal reaction kettle, maintenance hydrothermal temperature is 56 DEG C of hydro-thermal reaction 32min, and product is transferred in reaction kettle, is stirred
Speed is 150r/min, and 123 DEG C of maintenance system temperature, -0.06MPa are evaporated under reduced pressure 1h, by 5.1 parts of 2- acrylamide -2- methyl
Propane sulfonic acid is added to reaction kettle, mixing speed 115r/min, and maintenance system reaction temperature is 129 DEG C, -0.07MPa is depressurized back
Stream reaction 3.5h, product are evaporated under reduced pressure 1.5h through 135 DEG C, -0.08MPa, and product is washed through 800mL water washing 3 times, 350mL ethyl alcohol
It washs 2 times, dry to get 2- acrylamide-2-methyl propane sulfonic modified pitch is arrived；
(5), 76 parts of acrylate pre-emulsions and 6.5 parts of modified pitch are added in reaction kettle, mixing speed 110r/
Min reacts 25min under the conditions of 30 DEG C of maintenance system temperature, by 5 parts of 2- acrylamide-2-methyl propane sulfonic modified pitch and
The mixed liquor of 12.7 parts of hydroxypropyl acrylate modified pitch is added in reaction kettle with the adding rate of 0.2 part/min, in maintenance
The 40min that states under reaction condition that the reaction was continued, is warming up to 80 DEG C of reaction 3.5h for temperature of reaction kettle, temperature of reaction kettle is cooled to 50
DEG C, the 20min that maintains under the conditions of above-mentioned mixing speed that the reaction was continued is to get to asphalt modification water-proof emulsion.
Reference examples 1
In this reference examples, modified pitch is not added, other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, hydroxypropyl acrylate modified pitch, other components and preparation method and 1 phase of embodiment are not added
Together.
Reference examples 3
In this reference examples, do not add 2- acrylamide-2-methyl propane sulfonic modified pitch, other components and preparation method with
Embodiment 1 is identical.
Reference examples 4
The modified pitch in plain asphalt alternate embodiment 1, other components and preparation side are selected in this reference examples, in formula
Method is same as Example 1.
Reference examples 5
The acrylate pre-emulsion in conventional propylene acid butyl ester alternate embodiment 1 is selected in this reference examples, in formula, it is other
Component is same as Example 1 with preparation method.
Reference examples 6
The hydroxypropyl acrylate modified pitch in plain asphalt alternate embodiment 1 is selected in this reference examples, in formula, it is other
Component is same as Example 1 with preparation method.
Reference examples 7
In this reference examples, the 2- acrylamide-2-methyl propane sulfonic in plain asphalt alternate embodiment 1 is selected to change in formula
Property pitch, other components and preparation method are same as Example 1.
To asphalt modification water-proof emulsion, waterproof performance and tensile strength made from Examples 1 to 8 and reference examples 1~8 according to
JC/T 547-2017 is tested, and test result sees below Tables 1 and 2.
The performance parameter of asphalt modification water-proof emulsion made from 1 Examples 1 to 8 of table
Waterproof performance is evaluated by immersion time of whitening after emulsion film forming.
The performance parameter of asphalt modification water-proof emulsion made from 2 embodiment 1 of table and reference examples 1~8
By upper Tables 1 and 2 it is found that the waterproof and stretching of the asphalt modification water-proof emulsion that various embodiments of the present invention are prepared
It has excellent performance, this shows that the asphalt modification water-proof emulsion being prepared with raw material provided by the invention has excellent waterproof and drawing
Stretch performance；In contrast, the waterproof and tensile property for the asphalt modification water-proof emulsion that the raw material of each reference examples is prepared are poor.
In addition, the asphalt modification water-proof emulsion that various embodiments of the present invention are prepared has excellent waterproof and tensile property.
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art
For, under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as
The protection scope of the invention.
Claims (3)
1. a kind of asphalt modification water-proof emulsion, which is characterized in that by mass parts ratio be 5:7~16:68~83:3~8 2- third
Acrylamide -2- methyl propane sulfonic acid modified pitch, hydroxypropyl acrylate modified pitch, acrylate pre-emulsion and modified pitch group
At；Wherein, the 2- acrylamide-2-methyl propane sulfonic modified pitch is 12:35~41:27~36 by mass parts ratio:
18~26:2~7:2~8 pitch, toluene, dimethylbenzene, hydrogen peroxide, SE-10 emulsifier and 2- acrylamide -2- methyl-prop
Sulfonic acid reaction is made；The hydroxypropyl acrylate modified pitch is 16:8~17:6~14:43~55 by mass parts ratio
Pitch, maleic anhydride, hydroxypropyl acrylate and toluene reaction are made；The acrylate pre-emulsion is by mass parts ratio
4:16~23:14~22:8~15:4~9:2~5:0.3~1:39~58:1~7 acrylic acid, butyl acrylate, acrylic acid
Different monooctyl ester, 2-ethyl hexyl acrylate, 2- acrylamide-2-methyl propane sulfonic, AE-320 reactive emulsifier, ammonium persulfate, water and
The reaction of APE-2012 reactive emulsifier is made；The modified pitch by mass parts ratio be 10:9~15:4~12:6~
It is the pitch of 11:0.3~1:60~65, maleic anhydride, polyethylene glycol 400, polytetrahydrofuran ether glycol PTMEG250, anhydrous
Aluminium chloride and dimethylbenzene reaction are made.
2. asphalt modification water-proof emulsion according to claim 1, which is characterized in that the 2- acrylamide -2- methyl-prop
Sulfonic acid modified pitch, hydroxypropyl acrylate modified pitch, acrylate pre-emulsion and modified pitch mass parts ratio be 5:
9.8:75:4.9。
3. the preparation method of any asphalt modification water-proof emulsion of claim 1~2, which comprises the steps of:
(1), pitch and maleic anhydride are added in mixer, it is close under the conditions of 107~145 DEG C of maintenance system smelting temperature
15~50min is refined, product is through 50 DEG C of 500mL water supersound washing 3 times, drying, by product and polyethylene glycol 400, polytetrahydrofuran
Ether glycol PTMEG250, anhydrous aluminum chloride and toluene are added in reaction kettle, mixing speed 98r/min, reaction temperature 128
~136 DEG C, -0.06MPa reduced-pressure backflow 1~4h of reaction, product are evaporated under reduced pressure 1.5h, product warp through 143 DEG C, -0.09MPa
500mL ether wash 3 times, it is 500mL ethanol washing 3 times, dry, obtain modified pitch；
(2), by acrylic acid, butyl acrylate, Isooctyl acrylate monomer, 2-ethyl hexyl acrylate, 2- acrylamide-2-methyl propane sulfonic,
AE-320 reactive emulsifier, 1/4 ammonium persulfate of ammonium persulfate mass fraction total amount, water and the emulsification of APE-2012 response type
Agent is added in reaction kettle, mixing speed 76r/min, and 0.5~2h is reacted under the conditions of 68~78 DEG C of maintenance system reaction temperature,
Temperature of charge is cooled to 40 DEG C, remaining ammonium persulfate is added in reaction kettle, maintains to continue under above-mentioned stirring condition anti-
35min is answered, acrylate pre-emulsion is obtained；
(3), pitch, maleic anhydride and toluene are added in reaction kettle, mixing speed 100r/min, maintenance system is anti-
Answering temperature is 129~145 DEG C of 0.5~2h of reaction, product through 55 DEG C of 650mL water washing 4 times, 500mL ethanol washing 2 times, do
It is dry, product and hydroxypropyl acrylate are added in reaction kettle, mixing speed 120r/min, maintenance system reaction temperature is
117~128 DEG C, -0.05MPa react 1.5~5h, product is through 750mL water washing 3 times, 300mL ethanol washing 2 times, dry, i.e.,
Obtain hydroxypropyl acrylate modified pitch；
(4), pitch, toluene, dimethylbenzene, hydrogen peroxide and SE-10 emulsifier are added in hydrothermal reaction kettle, maintain hydro-thermal anti-
Answering temperature is 49~63 DEG C of 13~41min of hydro-thermal reaction, product is transferred in reaction kettle, mixing speed 150r/min, is tieed up
123 DEG C of system temperature, -0.06MPa vacuum distillation 1h are held, 2- acrylamide-2-methyl propane sulfonic is added to reaction kettle, is stirred
Speed is 115r/min, and maintenance system reaction temperature is 119~132 DEG C, -0.07MPa reduced-pressure backflow reacts 2~6h, product warp
135 DEG C, -0.08MPa be evaporated under reduced pressure 1.5h, product is through 800mL water washing 3 times, 350mL ethanol washing 2 times, dry to get arriving
2- acrylamide-2-methyl propane sulfonic modified pitch；
(5), acrylate pre-emulsion and modified pitch are added in reaction kettle, mixing speed 110r/min, maintenance system
25min is reacted under the conditions of 30 DEG C of temperature, by 2- acrylamide-2-methyl propane sulfonic modified pitch and the modified drip of hydroxypropyl acrylate
Green mixed liquor is added in reaction kettle with 0.2 mass parts/min adding rate, maintains under above-mentioned reaction condition that the reaction was continued
Temperature of reaction kettle is warming up to 72~86 DEG C of 1.5~5h of reaction by 40min, and temperature of reaction kettle is cooled to 50 DEG C, remains above-mentioned and stirs
The 20min that mixes under velocity conditions that the reaction was continued is to get to asphalt modification water-proof emulsion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116063811A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Modified asphalt stabilizer for improving storage stability |
| PL443606A1 (en) * | 2023-01-27 | 2024-07-29 | Politechnika Lubelska | Method of modifying asphalt binders with a two-component polymer additive |
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| CN106883628A (en) * | 2017-04-18 | 2017-06-23 | 无锡市城市道桥科技有限公司 | A kind of preparation method of warm mix foamed asphalt |
| CN106893490A (en) * | 2017-03-23 | 2017-06-27 | 北京东方雨虹防水技术股份有限公司 | A kind of modified emulsion of emulsion type asphalt paint and preparation method thereof and coating |
| CN108485450A (en) * | 2018-04-12 | 2018-09-04 | 金华联创塑粉科技有限公司 | A kind of timber polyacrylic acid coating and preparation method thereof |
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| JPH03124786A (en) * | 1989-10-11 | 1991-05-28 | Kanebo N S C Kk | Pressure-sensitive adhesive emulsion composition and kraft tape prepared therefrom |
| CN103642393A (en) * | 2013-11-28 | 2014-03-19 | 宋传松 | Waterproof paint for roads and bridges and preparation method thereof |
| CN106893490A (en) * | 2017-03-23 | 2017-06-27 | 北京东方雨虹防水技术股份有限公司 | A kind of modified emulsion of emulsion type asphalt paint and preparation method thereof and coating |
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| CN116063811A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Modified asphalt stabilizer for improving storage stability |
| PL443606A1 (en) * | 2023-01-27 | 2024-07-29 | Politechnika Lubelska | Method of modifying asphalt binders with a two-component polymer additive |
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