CN102276790B - Method for preparing bulking agent of epoxy resin modified asphalt - Google Patents
Method for preparing bulking agent of epoxy resin modified asphalt Download PDFInfo
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- CN102276790B CN102276790B CN 201110228109 CN201110228109A CN102276790B CN 102276790 B CN102276790 B CN 102276790B CN 201110228109 CN201110228109 CN 201110228109 CN 201110228109 A CN201110228109 A CN 201110228109A CN 102276790 B CN102276790 B CN 102276790B
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Abstract
The invention relates to a method for preparing a bulking agent of epoxy resin modified asphalt. Epoxy resin modified asphalt material is applicable to pavement of a high-grade road, pavement of steel bridge deck and the like. The method for preparing the bulking agent of the epoxy resin modified asphalt is characterized by comprising the following steps of: 1) selecting the following raw materials in parts by weight: 100 parts of fatty acid, 150-250 parts of epoxy resin, 3-4 parts of catalyst and 580-610 parts of organic solvent for spare use; and 2) dispersing the fatty acid and the epoxy resin into the organic solvent, and adding the catalyst, and heating for 3-5 hours at the temperature of 100-150 DEG C so as to obtain the bulking agent of the epoxy resin modified asphalt. The bulking agent prepared by the method provided by the invention can cause mixing of asphalt and the epoxy resin to be more uniform.
Description
Technical field
The present invention relates to a kind of structure material, be specifically related to a kind of preparation method of expanding material of epoxy resin modified asphalt.Epoxy resin modified asphalt materials for highway is applicable to mating formation of advanced road, the mating formation etc. of Steel Bridge Deck.
Background technology
Pitch is important architectural waterproof material and material of construction, and engineering generally comes from the byproduct of refining of petroleum with pitch, and it is a kind of thermoplastic material, and is cheap and easy to get, is widely used in communications and transportation, agricultural, hydro project, industry, the department such as civilian.There is not the asphalt applications of modification when road pavement, because its temperature sensitivity is strong, easily aging, can soften stickness during high temperature, the contraction owing to internal stress during low temperature can crack, simultaneously because its cohesive force is not high, hardness is inadequate, after repeatedly rolling, can form rut, cheat the pavement diseases such as groove, affected the work-ing life on road surface.Therefore, pitch carries out modification to it as last using.
Method of modifying commonly used is that some organic or inorganic fillers and pitch are carried out mix, and properties-correcting agent commonly used has SBS, PE, EVA, waste old etc.In these methods, SBS is the most a kind of properties-correcting agent of present domestic and international application, because its brittle point temperature is very low, low-temperature performance is good.Viscosity is very large at normal temperatures, can resist rut, and then viscosity reduces rapidly when high temperature, has good workability, and these character all are the performances that desirable pitch has.But studies show that, these properties-correcting agent just hold altogether with pitch, just combine with Intermolecular Forces, rather than connect with chemical bond, and this has just caused the performance heterogeneity of pitch after the modification, poor storage stability, the problems such as easy segregation.
Chemical modification method generally is by adding expanding material, the additives such as relational extender make occur between polymkeric substance and pitch or pitch and the pitch related, the chemical reactions such as grafting, thereby form networked one-piece construction, wherein the performance of epoxy resin modified asphalt is very outstanding, Resins, epoxy is mixed with pitch, can form irreversible cross-linked network cured article after adding solidifying agent curing, its intensity is high, rigidity is large, it is 3～4 times of plain asphalt compound that curved under the normal temperature draws stiffness modulus, anti-fatigue performance is 10～30 times of asphalt concrete, has in addition acid and alkali-resistance, the dirty premium properties that waits of oil resistant.
But owing to the greatest differences that exists between the Resins, epoxy, pitch and the curing agent component that participate in blend on chemical structure, polarity, surface tension, the molecular weight, this species diversity causes the mixture generation to divide mutually.In addition, the specific inductivity of Resins, epoxy (bisphenol A-type) specific inductivity and petroleum pitch differs greatly equally.
So, use Resins, epoxy to asphalt modification, generally will carry out modification to pitch, but the pitch kind of using in this case and the polymkeric substance that is used for modification must be specific, have limited the development of thermoset pitch, another kind of method is the cosolvent method.Both employing and Resins, epoxy and petroleum pitch consistency third phases preferably all, it can reduce Resins, epoxy and petroleum pitch interfacial tension, when the two mixes, promotes the dispersion of pitch, stop the cohesion of pitch particle, and strengthen pitch particle and the macromolecular bonding of Resins, epoxy.In CN1546571, provided the epoxy bitumen material that comprises the modification of usefulness polyisobutylene butanedioic anhydride that a kind of motorway and bridge are used.In CN1952012, provided thermosetting epoxy asphalt material that a kind of use contains the mannich base of the senior fatty carbon chain of low-pole and strong polarity or Resins, epoxy and the dedicated compatibilizer modification of the epoxy bitumen material of the compound of polyvalent alcohol composition, it must not carry out chemical modification to pitch, do not need to limit the kind of pitch yet, only need in pitch, add dedicated compatibilizer, cooperate conventional Resins, epoxy and solidifying agent just can form thermosetting epoxy asphalt material.In CN101003688, provided relate to a kind of with pitch, solidifying agent, promotor, the high performance pavement material of epoxy asphalt that defoamer forms.It has good solidity to corrosion, water tolerance, weathering resistance, resistance to fatigue, high temperature creep resistant and low temperature resistance to brittle fracture.In CN101020601, provided a kind of poured epoxytar laying of roadway material with modification alkylphenol, glycidyl ether modified.It is a kind ofly have that construction temperature is low, good fluidity, the easily poured epoxytar concrete material of constructing.USP6399680 has provided with the sulfuric acid of the 0.02-3% of modifying asphalt total amount, phosphoric acid, Glacial acetic acid or nitric acid and has done promotor, contains the modifying asphalt that the multipolymer of epoxy group(ing) of the 0.2-15% of modifying asphalt total amount is made; Provided the method with polyamines and epoxy resin modified asphalt among the USP4162998; USP5576363 has provided the method for preparing the two-pack modified asphalt material with modifications such as the multipolymer that contains epoxide group and carboxylic acids; USP4360608 has provided with pitch, the epoxy bitumen material that Resins, epoxy and polyether glycol expanding material form, and as road surfacing material, it has preferably thermal deformation resistant ability and trickling property.Provided the modifying asphalt that the polymkeric substance of the modifying asphalt that contains the mineral acid group and linearity or branching prepares among the USP5095055, the road surface of laying this kind material has the visco-elasticity of the property improved, and softening temperature raises, the storage-stable property improvement.Provided the polymer modified asphalt material that total amount 0.1-5% contains epoxide group among the USP5306750, the polymkeric substance that contains epoxide group forms external phase in pitch, obtain thus having anti-rut, low temperature cracking resistance, the thermosetting modification pitch of anti-flexible fracture and moisture resistant destructiveness.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of expanding material of epoxy resin modified asphalt, the expanding material of the method preparation can make the mixing of pitch and Resins, epoxy more even.
To achieve these goals, the technical solution used in the present invention is: the preparation method of the expanding material of epoxy resin modified asphalt is characterized in that it comprises the steps:
1) by the shared parts by weight of each raw material be: 100 parts in lipid acid, Resins, epoxy 150-250 part, catalyzer 3-4 part, organic solvent 580-610 part, choose lipid acid, Resins, epoxy, catalyzer and organic solvent, for subsequent use;
2) lipid acid and Resins, epoxy are distributed in the organic solvent, and add catalyzer, 100-150 ℃ of heating 3-5 hour, obtain the expanding material (it is to contain the higher fatty acid carbochain of two keys and the affixture of Resins, epoxy) of epoxy resin modified asphalt.
Described lipid acid is ricinolic acid, or contains the unsaturated fatty acids of 16-22 carbon atom, can be the mixture of two or more unsaturated fatty acids, is any proportioning between the unsaturated fatty acids in the mixture.
The described unsaturated fatty acids that contains the 16-22 carbon atom is specially oleic acid or undecylenic acid etc.
Described Resins, epoxy is bisphenol A type epoxy resin.
Described bisphenol A type epoxy resin is Resins, epoxy E-41, Resins, epoxy E-42, epoxy resin E-44 or Resins, epoxy E-51.
Described catalyzer is the anionic catalysts such as inorganic salt, mineral alkali or amine.
Described inorganic salt anionic catalyst is CaCl
2
Described mineral alkali anionic catalyst is LiCl or LiOH.
Described amine anionic catalyst is Tetrabutyl amonium bromide, triethylamine or quadrol.
Described organic solvent is the organic solvents such as chloroform, benzene (not comprising toluene) or toluene.
The general molecular formula of the expanding material of resulting epoxy resin modified asphalt is as follows:
Senior fatty carbon chain is ricinolic acid, or contains the unsaturated fatty acids of 16-22 carbon atom, can be the mixture of two or more unsaturated fatty acids.
The concrete structure formula is as follows:
Wherein A is the dihydroxyphenyl propane group.
In the technique scheme, the Resins, epoxy group is the bisphenol A epoxide resin group, and senior fatty carbon chain is unsaturated fatty acids.
The application of expanding material of the present invention: use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the expanding material of the vulcanizing agent of the solidifying agent of the Resins, epoxy of the pitch of 100 parts of weight, 20-40 part weight, 20-40 part weight, 2.0-10 part weight and 20-60 part weight is mixed, be heated to 100-150 ℃ of heating 2-9h, obtain epoxy resin modified asphalt.The present invention can add 1000 parts of building stones in the epoxy resin modified asphalt preparation of (or claiming thermoset pitch), further increase its intensity.
Described pitch is petroleum pitch or coal-tar pitch.Petroleum pitch comprises 70
#, 90
#, 100
#National highway, one-level road, town and country bitumen for road use, SBS modifying asphalt, 10
#Building materials pitch, 2 discharges water
#Pipeline corrosion protection pitch.
Described Resins, epoxy is epoxy resin E-44, Resins, epoxy E-51, Resins, epoxy E-42 or Resins, epoxy E-41.
Described solidifying agent is amine curing agent, acid anhydride type curing agent, or the solidifying agent that cooperates of amine and anhydrides.Amine curing agent such as diethylenetriamine, quadrol, m-xylene diamine etc., acid anhydride type curing agent such as Tetra hydro Phthalic anhydride, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride etc.
Described pitch vulcanizing agent vulcanization crosslinking.Vulcanizing agent is sulphur and smog inhibitor zinc Synergist S-421 95, and the mass ratio of sulphur and smog inhibitor zinc is 1000: 1; Or vulcanization accelerator tetramethyl-thiuram disulfide.
The action principle of the expanding material of epoxy resin modified asphalt of the present invention is as follows: the expanding material of epoxy resin modified asphalt is that an end contains the higher unsaturated fatty acid of low-pole and the compound that the other end contains epoxide group.The compatibilization of expanding material in pitch and Resins, epoxy is similar to the emulsifying effect of tensio-active agent in You Heshui.Senior fatty carbon chain and the pitch of low-pole is more affine in the expanding material molecule, and the strong part of polarity is more affine with Resins, epoxy, thereby reach the purpose that pitch and Resins, epoxy can mix more equably, in addition, contain the unsaturated fatty acids carbochain of two keys after sulfuration, can with pitch in unsaturated double-bond carry out crosslinked, the epoxide group of the other end is after solidifying and cross linking of epoxy resin, such three kinds of components with mutual biography network connection together, thereby play stable modification pitch chemical property, improve the purpose of pitch overall performance.
The present invention compared with prior art has following beneficial effect:
1, the expanding material of the method preparation mixing more evenly (expanding material can make Resins, epoxy and pitch better compatible) that can make pitch and Resins, epoxy.
2, the present invention is simple to operate, and is with low cost, do not need the direct modification of pitch, enlarged the pitch kind, only need in pitch, to add expanding material, cooperate again conventional Resins, epoxy and solidifying agent thereof, form thermosetting epoxy asphalt, its intensity is high, and rigidity is large, and good use properties is arranged.
3, in the epoxy resin modified asphalt of the present invention, owing to adding expanding material, described epoxy resin ingredient is applicable to most Resins, epoxy, such as the glycidyl ether based epoxy resin, the glycidyl ester based epoxy resin, Racemic glycidol amine epoxy resin, aliphatic category Resins, epoxy or cycloaliphatic epoxy resin, so that the raw material selectable range of the epoxy resin modified asphalt of preparation enlarges, provide wide selection space for reducing cost like this.
4, the senior fatty carbon chain of expanding material of the present invention partly is unsaturated fatty acids, and polar portion is Resins, epoxy.Vulcanization reaction can occur with pitch in unsaturated group under the effect of vulcanizing agent, curing reaction can occur with Resins, epoxy in epoxy group(ing) under the effect of solidifying agent and curing catalyst, can make pitch like this, Resins, epoxy, the expanding material three forms the three-dimensional crosslinked network structure of an IPN.And existing thermoset pitch preparation method CN1950212 has prepared a kind of expanding material, this expanding material is that the form with disperse phase distributes wherein equably in pitch, between pitch and Resins, epoxy, play an instrumentality, to reduce the interfacial tension at Resins, epoxy and pitch two interfaces.
Description of drawings
Fig. 1 is gained expanding material infared spectrum in the embodiment of the invention 1.
Fig. 2 is in the embodiment of the invention 1 used 70
#The pitch infared spectrum.
Fig. 3 is the infared spectrum of gained epoxy resin modified asphalt in the embodiment of the invention 1.
Fig. 4 a is the scanning electron photomicrograph (3000X) of epoxy resin modified asphalt in the embodiment of the invention 1.
Fig. 4 b is the scanning electron photomicrograph (10000X) of epoxy resin modified asphalt in the embodiment of the invention 1.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
In constant temperature oil bath, add 100 gram ricinolic acids, 155 gram E-44 Resins, epoxy, 595 gram trichloromethanes, 3.1 gram Tetrabutyl amonium bromides, heating up causes 100 ℃ of reactions 3 hours, steams solvent (trichloromethane), obtains the expanding material of epoxy resin modified asphalt.
The expanding material of resulting epoxy resin modified asphalt, its structural formula comprises following structure:
Wherein, A is the dihydroxyphenyl propane group.
The expanding material that the present embodiment arrives is used the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, and it comprises the steps:
The expanding material, 2 that No. 70 pitches of 100 gram shell, 35 gram epoxy resin E-44s, 40 gram the present embodiment are arrived restrains sulphur (vulcanizing agent), the inhibitor (zinc hydroxyl stannate) 0.002 gram is fuming, 30 gram methyl hexahydrophthalic anhydrides, being heated to 80 ℃ stirs, 100 ℃ of lower 2h that solidify, then at 150 ℃ of lower 7h that solidify, get epoxy resin modified asphalt.
In the embodiment of the invention 1 gained expanding material infared spectrum as shown in Figure 1, by shown in Figure 1 at 3340cm
-1The place is-the OH stretching vibration peak 2944cm
-1The place is aromatic C-H or CH
2Stretching vibration, 1606cm
-1Be the two key stretching vibrations of phenyl ring skeleton C=C, 828cm
-1The stretching vibration of epoxy group(ing), 728cm
-1Be the flexural vibration peak of C-H among the-C=C-, 1742cm
-1Be the two key stretching vibrations of C=O, 1190cm
-1Be the stretching vibration peak of-C-O-C-, illustrated that ester group generates.Have epoxy group(ing) and-COOH reaction descriptions reaction is carried out smoothly, and final expanding material comprises our needed pair of key group and epoxide group.
Used 70
#The pitch infared spectrum as shown in Figure 2.In the embodiment of the invention 1 infared spectrum of gained epoxy resin modified asphalt as shown in Figure 3, as seen from Figure 3,1740cm
-1, 1710cm
-1Near absorption peak is the C=O absorption peak, new wave band occurs at this two place, owing to having generated ester bond and carboxylic acid in the Curing Process of Epoxy.1250cm
-1, 1183cm
-1It is bimodal that the place presents, and is the absorption peak of two aryl oxides and bis-phenol ether, 1041cm
-1Place's bands of a spectrum are the absorption peak of fatty ether, and these several structures can find in the structural formula of expanding material.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, shown in Fig. 4 a and Fig. 4 b, Fig. 4 a and Fig. 4 b have illustrated: Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 2:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
In constant temperature oil bath, add 100 gram ricinolic acids, 155 gram E-41 Resins, epoxy, 595 gram trichloromethanes, 3.1 gram Tetrabutyl amonium bromides, heating up causes 100 ℃ of reactions 3 hours, steams solvent (trichloromethane), obtains the expanding material of epoxy resin modified asphalt.
The expanding material of resulting epoxy resin modified asphalt, its structural formula comprises following structure:
Wherein, A is the dihydroxyphenyl propane group.
The expanding material that the present embodiment arrives is used the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, and it comprises the steps:
The expanding material, 2 that No. 90 pitches of 100 gram shell, 35 gram epoxy resin E-44s, 40 gram the present embodiment are arrived restrains vulcanizing agents (sulphur), the inhibitor (zinc hydroxyl stannate) 0.002 gram is fuming, 30 gram methyl hexahydrophthalic anhydrides, being heated to 80 ℃ stirs, 100 ℃ of lower 2h that solidify, then at 150 ℃ of lower 7h that solidify, get epoxy resin modified asphalt.
The present invention can add 10000 gram building stones in the preparation of epoxy resin modified asphalt, can further increase its intensity.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 3:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
100 gram oleic acid and 160 gram E-41 Resins, epoxy are distributed in the 606 gram organic solvents, chloroforms, and add 3.2 gram catalyzer (inorganic salt anionic catalyst, CaCl
2), 100 ℃ of heating 3 hours, obtain the expanding material of epoxy resin modified asphalt.
The application of expanding material of the present invention: use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the vulcanizing agent tetramethyl-thiuram disulfide of the solidifying agent diethylenetriamine of the Resins, epoxy E-41 of No. 70 pitches of 100 gram shell, 20 grams, 20 grams, 4 grams and the expanding material of 20 grams are mixed, being heated to 80 ℃ stirs, 100 ℃ of lower 2h that solidify, then at 150 ℃ of lower 7h that solidify, obtain epoxy resin modified asphalt.The present invention can add 1000 gram building stones in the epoxy resin modified asphalt preparation of (or claiming thermoset pitch), can further increase its intensity.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 4:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
1) by the shared weight of each raw material be: oleic acid 100 grams, Resins, epoxy E-41 160 grams, catalyzer LiCl 3 grams, toluene 580 grams, choose oleic acid, Resins, epoxy E-41, catalyzer LiCl and toluene, for subsequent use;
2) oleic acid and Resins, epoxy E-41 are distributed in the toluene (organic solvent), and add catalyzer LiCl, 100 ℃ of heating 5 hours, obtain the expanding material of epoxy resin modified asphalt.
Use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the pitch (90 with 100 grams
#), the epoxy resin E-44s of 20 grams, the solidifying agent (diethylenetriamine) of 20 grams, the vulcanizing agents (tetramethyl-thiuram disulfide) of 2.1 grams and expanding materials (being the expanding material of the epoxy resin modified asphalt) mixing of 20 grams, be heated to 100 ℃ of heating 2h, obtain epoxy resin modified asphalt.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 5:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
1) by the shared weight of each raw material be: undecylenic acid 100 grams, Resins, epoxy E-42 250 grams, catalyzer LiOH 3.2 grams, benzene 610 grams, choose undecylenic acid, Resins, epoxy E-42, catalyzer LiOH and benzene (organic solvent), for subsequent use;
2) undecylenic acid and Resins, epoxy E-42 are distributed in the organic solvent-benzene, and add catalyzer LiOH, 150 ℃ of heating 5 hours, obtain the expanding material of epoxy resin modified asphalt.
Use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the pitch (100 with 100 grams
#National highway), the expanding materials of the vulcanizing agents of the solidifying agent (quadrol) of the Resins, epoxy E-51 of 40 grams, 40 grams, 10 grams and 60 grams (being the expanding material of the epoxy resin modified asphalt that obtains of the present embodiment) mix, be heated to 150 ℃ of heating 9h, obtain epoxy resin modified asphalt.
Vulcanizing agent is sulphur and smog inhibitor zinc Synergist S-421 95, and the mass ratio of sulphur and smog inhibitor zinc is 1000: 1.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 6:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
1) by the shared weight of each raw material be: undecylenic acid 100 grams, Resins, epoxy E-51 211 grams, triethylamine (catalyzer) 3 grams, chloroform (organic solvent) 600 grams, choose undecylenic acid, Resins, epoxy E-51, triethylamine and chloroform, for subsequent use;
2) undecylenic acid and Resins, epoxy E-51 are distributed in the chloroform (organic solvent), and add triethylamine (catalyzer), 100 ℃ of heating 4 hours, obtain the expanding material of epoxy resin modified asphalt.
Use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the vulcanizing agents (tetramethyl-thiuram disulfide) of the solidifying agent (m-xylene diamine) of the Resins, epoxy E-42 of the pitches (SBS modifying asphalt) of 100 grams, 30 grams, 30 grams, 5 grams and the expanding materials of 40 grams (being the expanding material of the epoxy resin modified asphalt that obtains of the present embodiment) mixing, be heated to 130 ℃ of heating 6h, obtain epoxy resin modified asphalt.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Embodiment 7:
The preparation method of the expanding material of epoxy resin modified asphalt, it comprises the steps:
1) by the shared weight of each raw material is: oleic acid and undecylenic acid 100 grams (each 50 gram of oleic acid and undecylenic acid), Resins, epoxy E-51 150 grams, quadrol 4 grams, chloroform 580 grams, choose oleic acid, undecylenic acid, Resins, epoxy E-51, quadrol and chloroform, for subsequent use;
2) oleic acid, undecylenic acid, Resins, epoxy E-51 have been distributed in the chloroform, and have added quadrol, 150 ℃ of heating 3 hours, obtained the expanding material of epoxy resin modified asphalt.
Use the preparation epoxy resin modified asphalt, the preparation method of epoxy resin modified asphalt, it comprises the steps: the vulcanizing agents (tetramethyl-thiuram disulfide) of the solidifying agent (m-xylene diamine) of the Resins, epoxy E-42 of the pitches (SBS modifying asphalt) of 100 grams, 30 grams, 30 grams, 5 grams and the expanding materials of 40 grams (being the expanding material of the epoxy resin modified asphalt that obtains of the present embodiment) mixing, be heated to 130 ℃ of heating 6h, obtain epoxy resin modified asphalt.
Microtexture with sem observation hot epoxy resin modifying asphalt, the SEM photo shows, Resins, epoxy, pitch, three kinds of components of expanding material can form cross-linked network, solidification effect is desirable, illustrate that the expanding material that the method obtains can make the mixing of pitch and Resins, epoxy more even (expanding material can make Resins, epoxy and pitch better compatible).
Each raw material that the present invention is cited, and the bound of each raw material of the present invention, interval value, and the bound of processing parameter (such as temperature, time etc.), interval value can both realize the present invention, do not enumerate one by one embodiment at this.
Claims (3)
1. the preparation method of the expanding material of epoxy resin modified asphalt is characterized in that it comprises the steps:
1) by the shared parts by weight of each raw material be: 100 parts in lipid acid, Resins, epoxy 150-250 part, catalyzer 3-4 part, organic solvent 580-610 part, choose lipid acid, Resins, epoxy, catalyzer and organic solvent, for subsequent use;
Described lipid acid is ricinolic acid; Or contain the unsaturated fatty acids of 16-22 carbon atom, and be the mixture of two or more unsaturated fatty acids, be any proportioning between the unsaturated fatty acids in the mixture;
Described catalyzer is inorganic salt, mineral alkali or amine anionic catalyst;
Described inorganic salt anionic catalyst is CaCl
2
Described mineral alkali anionic catalyst is LiCl or LiOH;
Described amine anionic catalyst is Tetrabutyl amonium bromide, triethylamine or quadrol;
2) lipid acid and Resins, epoxy are distributed in the organic solvent, and add catalyzer, 100-150 ℃ of heating 3-5 hour, obtain the expanding material of epoxy resin modified asphalt.
2. the preparation method of the expanding material of epoxy resin modified asphalt according to claim 1, it is characterized in that: described Resins, epoxy is bisphenol A epoxide resin.
3. the preparation method of the expanding material of epoxy resin modified asphalt according to claim 1, it is characterized in that: described organic solvent is chloroform, benzene or toluene.
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| CN116041670A (en) * | 2022-12-20 | 2023-05-02 | 江苏扬农锦湖化工有限公司 | Acid modified epoxy resin and preparation method and application thereof |
| CN117050541B (en) * | 2023-07-27 | 2024-05-28 | 山东百成新材料科技股份有限公司 | High-temperature-resistant composite modified asphalt for highway and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1952012A (en) * | 2006-10-20 | 2007-04-25 | 中国林业科学研究院林产化学工业研究所 | Thermosetting epoxy asphalt material, preparation method and its dedicated compatibilizer |
| CN101955675A (en) * | 2010-10-18 | 2011-01-26 | 武汉工程大学 | Modified epoxy resin thermosetting epoxy asphalt bulking agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1952012A (en) * | 2006-10-20 | 2007-04-25 | 中国林业科学研究院林产化学工业研究所 | Thermosetting epoxy asphalt material, preparation method and its dedicated compatibilizer |
| CN101955675A (en) * | 2010-10-18 | 2011-01-26 | 武汉工程大学 | Modified epoxy resin thermosetting epoxy asphalt bulking agent and preparation method thereof |
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