CN104877357A - Preparation method and application of epoxy asphalt compatibilizer - Google Patents
Preparation method and application of epoxy asphalt compatibilizer Download PDFInfo
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- CN104877357A CN104877357A CN201510234752.9A CN201510234752A CN104877357A CN 104877357 A CN104877357 A CN 104877357A CN 201510234752 A CN201510234752 A CN 201510234752A CN 104877357 A CN104877357 A CN 104877357A
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Abstract
The invention relates to a preparation method of an epoxy asphalt compatibilizer, which comprises the following steps: a) heating heavy aromatic oil to 60-180 DEG C; and b) adding isocyanate accounting for 3-10 wt% of the heavy aromatic oil, 0.5-5 wt% of initiator and 3-10 wt% of anti-degradant into the heavy aromatic oil, and stirring for 0.5-2 hours to obtain the epoxy asphalt compatibilizer. The epoxy asphalt compatibilizer obtained by the method can increase the compatibility between the matrix asphalt and epoxy resin. The application method of the epoxy asphalt compatibilizer comprises the following steps: adding asphalt, the epoxy asphalt compatibilizer, an epoxy asphalt diluter, an epoxy resin and an epoxy resin diluter into a reaction kettle, and mixing to obtain a part A of the epoxy asphalt material; and mixing the part A of the epoxy asphalt material with a part B epoxy asphalt curing agent of the epoxy asphalt material to obtain the epoxy asphalt material applicable to room-temperature construction. The material can be directly laid on the pavement at room temperature, or mixed with aggregate stone and laid on the pavement.
Description
Technical field
The present invention relates to road new material technology field, particularly relate to and a kind ofly may be used for preparing the preparation and application of the expanding material of epoxy bitumen material that at room temperature can be uniformly mixed, construct.
Background technology
Compared with plain asphalt, epoxy bitumen material has the weather resistance of very excellent high-temperature stability, crack resistance at low-temperature, superpower anti-fatigue performance and excellence, becomes the preferred material in high paving steel bridge deck engineering.In the process preparing bituminous epoxy, main component due to bituminous epoxy PetroChina Company Limited. pitch is the mixture of fat hydrocarbon and arene, its solubility parameter is about 8.66, and the solubility parameter of epoxy resin is 10.36, therefore mixed system is thermodynamically difficult to compatible and becomes the system of stable homogeneous.In order to effectively prepare epoxy bitumen material, the compatibility problem between the matrix pitch of primary solution and epoxy resin.
On the other hand, epoxy bitumen material disclosed in prior art is at room temperature semi-fluid paste, and must heat when mating formation and using, the temperature of mixing and stirring as U.S. ChemCo bituminous epoxy is 121 DEG C, and the temperature of mixing and stirring of Japanese TAF bituminous epoxy is 180 DEG C.And, bituminous epoxy through mixing and stirring gathers materials and under heat-retaining condition, must be transported to working-yard from blending station, cause on the one hand because external heat makes the production energy consumption of bituminous epoxy high like this, simultaneously large due to transport difficulty when heat insulation transportation causes construction must be carried out; Meanwhile, bituminous epoxy, in heat-processed, can produce harmful bitumen flue gas, causes larger impact to the health of constructor and environment.
Summary of the invention
The object of the present invention is to provide a kind of method of preparation and use of bituminous epoxy expanding material.Compatibility problem between the soluble matrix pitch of bituminous epoxy expanding material utilizing the technology of the present invention to obtain and epoxy resin, the epoxy bitumen material utilizing this bituminous epoxy expanding material to prepare at room temperature can be uniformly mixed, construct.
For achieving the above object, the technical solution used in the present invention is, a kind of preparation method of bituminous epoxy expanding material, is characterized in that comprising the following steps:
A) heavy aromatics oil is heated to 60 ~ 180 DEG C;
B) to attach most importance to by the consumption of isocyanic ester 3 ~ 10% of aromatic hydrocarbon oil parts by weight, the consumption of initiator is attached most importance to 0.5 ~ 5% of aromatic hydrocarbon oil parts by weight, the consumption of anti degradant is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, isocyanic ester, initiator and anti degradant mixed solution are joined in heavy aromatics oil, under the condition of heating, stir 0.5 ~ 2h, obtain bituminous epoxy expanding material.
Preferably, in described heavy aromatics oil, heavy aromatics content is 30 ~ 85% (quality), is more preferably 50 ~ 80%, is more preferably 60 ~ 75%.
Preferably, the Heating temperature of described heavy aromatics oil is 60 ~ 180 DEG C, is more preferably 80 ~ 160 DEG C, is more preferably 120 ~ 150 DEG C.
The present invention does not have special restriction to described heavy aromatics oil kind and source; adopt the kind of the heavy aromatics oil of those skilled in the art's accreditation and originate, as the heavy aromatics oil purchased from protecting magnificent petrochemical industry novel material exploitation limited-liability company purchased from Wuhan can be adopted.
Preferably, the consumption of described isocyanic ester is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, is more preferably 5 ~ 9%, is more preferably 6 ~ 8%.Described isocyanic ester can be at least one in tolylene diisocyanate, '-diphenylmethane diisocyanate, poly methylene poly phenyl poly isocyanate, the multiple mixing by any proportioning.The present invention does not have special restriction to described isocyanic ester kind and source, adopt the kind of the isocyanic ester of those skilled in the art's accreditation and originate, as the 3-sec.-propyl-alpha, alpha-dimethylbenzyl isocyanic ester (TMI) purchased from ALDRICH company can be adopted.
Preferably, the consumption of described initiator is attached most importance to 0.5 ~ 5% of aromatic hydrocarbon oil parts by weight, is more preferably 1 ~ 4%, is more preferably 1 ~ 3%.The present invention does not have special restriction to described initiator type and source, adopt the kind of the initiator of those skilled in the art's accreditation and originate, as can adopt purchased from Chengdu Li Jingxiwang Fine Chemical Co., Ltd 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DHBP).
Preferably, the consumption of described anti degradant is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, is more preferably 5 ~ 9%, is more preferably 6 ~ 8%.The present invention does not have special restriction to described anti degradant kind and source, adopts the kind of the anti degradant of those skilled in the art's accreditation and originates, as adopted the vinylbenzene (St) purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
In the present invention, bituminous epoxy expanding material effectively can improve the consistency between pitch and epoxy resin, makes the epoxy bitumen material of preparation have the phase of stable uniform, can not there is being separated of pitch and epoxy resin two-phase.Active group contained by bituminous epoxy expanding material provided by the present invention can participate in curing cross-linking reaction, forms the stronger more firmly molecular linkage of reactive force, more effectively to increase the consistency between pitch and epoxy resin; On the other hand, due to different from the reactive behavior of epoxy resin, cause reaction to interlock to carry out, thus form a kind of inierpeneirating network structure (IPN structure), and this network structure has overall cross-linking density is low, partial cross-linking density is high dual-mode network constitutional features, while bituminous epoxy can be made at high temperature to have high strength, at low temperatures also there is good toughness.
Invention also provides a kind of application of bituminous epoxy expanding material, it is characterized in that comprising the following steps:
1) pitch, bituminous epoxy expanding material, bituminous epoxy thinner, epoxy resin, epoxy resin diluent are joined in reactor together and be uniformly mixed, obtain the part A of epoxy bitumen material;
Described part A comprises the component of following weight part:
2) by described step 1) part A of epoxy bitumen material that obtains mixes with the part B agitating of epoxy bitumen material, obtain a kind of can the epoxy bitumen material of at room temperature construction usage.
Described part B comprises the component of following weight part:
20 ~ 50 parts, bituminous epoxy solidifying agent;
3) by step 2) described epoxy bitumen material is directly layed in road surface, or join after building stones mix with collection and be layed in road surface.
Building stones gathering materials as AC-10 is joined in described integrating, and the AC-10 preferably utilizing basalt to prepare gathers materials.
Described epoxy bitumen material and collection join the weight ratio of the bitumen aggregate ratio of building stones for (6.5 ~ 8): 100, are preferably (6.8 ~ 7.5): 100, are more preferably (6.8 ~ 7.2): 100.
Described pitch is preferably at least one in petroleum pitch, oxidized bitumen, coal-tar pitch, lake pitch, multiple by any proportioning mixing.The present invention does not have special restriction to described pitch kind and source, adopts the kind of the pitch of those skilled in the art's accreditation and originates, and is the shell pitch of No. 70 as adopted the trade mark.
Preferably, described step 1) agitating mixing time be 0.5 ~ 2h, step 2) in agitating mixing time be 0.2 ~ 1h.
Preferably, described step 1) agitating mixing temperature be room temperature ~ 180 DEG C, step 2) in agitating mixing temperature be room temperature.
Pitch, bituminous epoxy expanding material, bituminous epoxy thinner, epoxy resin, epoxy resin diluent first join in common reactor by the present invention together, at stirring 0.5 ~ 2h under the condition of room temperature ~ 180 DEG C, obtain the part A of epoxy bitumen material.Method provided by the invention joins in reaction vessel by directly disposable for each component; compared with adding with component each in part A disclosed in prior art in batches; method provided by the invention carries out high speed dispersion without the need to adopting special colloidal mill, more without the need to passing into nitrogen protection reaction or the complex operations of use condensate return a few hours.Method technology controlling and process provided by the invention is simple, and hold facility is few, as long as join directly disposable for each component of part A in common reactor, mixes and namely obtains part A.In the present invention, consistent with described in technique scheme of the kind of described pitch, bituminous epoxy expanding material, bituminous epoxy thinner and bituminous epoxy solidifying agent and weight ratio, does not repeat them here.
In the present invention, by weight, described part A comprises the bituminous epoxy expanding material of 10 ~ 50 parts, is preferably 15 ~ 45 parts, is more preferably 20 ~ 40 parts.Described bituminous epoxy expanding material is based on the judgement of solubility parameter with the similar principle that mixes, by the method for organic synthesis, the dicyclo contained in heavy aromatics, polynuclear plane are introduced the active function groups that curing cross-linked can occur, prepare a kind of response type bituminous epoxy expanding material forming the modification heavy aromatics of gelling system, this response type bituminous epoxy expanding material and common expanding material are just formed compared with Van der Waals force or hydrogen bond between the two phases, not only effectively pitch can be dispersed to micron order to hundred nano-scale; Simultaneously, because it contains the active function groups that curing cross-linked can occur, gelation reaction can be there is, the molecular linkage that reactive force is stronger is formed between pitch and epoxy resin, thermodynamically form the single phase of stable uniform with pitch, fundamentally improve the consistency between pitch and epoxy resin.
In the present invention, by weight, described part A comprises the bituminous epoxy thinner of 5 ~ 50 parts, is preferably 10 ~ 45 parts, is more preferably 20 ~ 40 parts; Preferably, described bituminous epoxy thinner is at least one in vinylbenzene, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, multiple by any proportioning mixing.The present invention does not have special restriction to described bituminous epoxy thinner kind and source, adopt the bituminous epoxy thinner kind of those skilled in the art's accreditation and originate, as the vinylbenzene (St) purchased from Chemical Reagent Co., Ltd., Sinopharm Group can be adopted.
By weight, described part A comprises the epoxy resin diluent of 5 ~ 50 parts, is preferably 10 ~ 45 parts, is more preferably 20 ~ 40 parts; Preferably, described epoxy resin diluent is styrene oxide, phenyl glycidyl ether, p-cresol glycidyl ether, 2-Racemic glycidol phenyl glycidyl ether, 2, at least one in 6-2-glycidyl phenyl glycidyl ether, o-phthalic acid diglycidyl ester, tetrahydrophthalic acid 2-glycidyl ester, hexahydrophthalic acid 2-glycidyl ester, multiple by any proportioning mixing.The present invention does not have special restriction to described epoxy resin diluent kind and source, adopting the epoxy resin diluent kind of those skilled in the art's accreditation and originate, is the glycidyl ether type epoxy thinner of 632 as adopted purchased from Yu Sheng Chemical Co., Ltd. of the Yantai City trade mark.
In the art, conventional thinner has gasoline, trichloromethane, the organic solvents such as benzene, the just physical dispersion (inertia dispersion) that this kind of thinner plays pitch, epoxy resin, namely just physical method is utilized, by pitch, epoxy resin from block lotion " decomposition " glomeration small-particle, the particle diameter after dispersion from grade to micron order not etc.; Simultaneously, such thinner is lower because of boiling point, finally can volatilize away from pitch, epoxy-resin systems, thus pitch, epoxy resin mutually in leave cellular pore space structure, form the rupture stress centrostigma of pitch, epoxy resin, finally cause dissociating of pitch, epoxy resin structural.
The bituminous epoxy thinner used in the present invention, epoxy resin diluent have high reactive behavior, long chain molecule structure can be generated by polymerization reaction take place, the cross-linked network structure of the bituminous epoxy prepared by optimizing further and mechanical property when not adding or add on a small quantity initiator.Namely, the bituminous epoxy thinner used in the present invention, epoxy resin diluent effectively can reduce the viscosity of bituminous epoxy, epoxy resin when the initial stage of use, increase the operability of construction, can cure-crosslinking agent be served as in the later stage used, improve consolidated structures and the mechanical property of bituminous epoxy.
Preferably, described epoxy resin is at least one in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, dihydroxyphenyl propane D type epoxy resin and resorcinol type epoxy, the multiple mixing by any proportioning.The source of the present invention to described epoxy resin does not have special restriction, can adopt the commercial goods of epoxy resin, is the epoxy resin of E-51 as adopted purchased from Ba Ling petrochemical industry limited liability company of the SINOPEC trade mark.
In the present invention, by weight, described part B comprises the bituminous epoxy solidifying agent of 20 ~ 50 parts, is preferably 20 ~ 40 parts, is more preferably 20 ~ 35 parts.In the present invention, described bituminous epoxy solidifying agent is at least one in fatty amines solidifying agent, alicyclic ring amine curing agent, aromatic amine curing agent, polyamide-based solidifying agent, multiple by any proportioning mixing.In the present invention, the molecular chain structure of described bituminous epoxy solidifying agent can form flexible portal structure between pitch and epoxy resin, improve physical strength and the stability of the bituminous material obtained, effectively improve the fragility of bituminous material, make the epoxy bitumen material obtained have higher toughness; Simultaneously, the bituminous epoxy solidifying agent used in the present invention is amine curing agent, has higher reactive behavior, can at relatively low temperatures with epoxy resin generation crosslinking reaction, higher solidification intensity can be formed in the short period, be conducive to the quick opening after road repair.The source of the present invention to described bituminous epoxy solidifying agent does not have special restriction, adopting the commercial goods of the bituminous epoxy solidifying agent of those skilled in the art's accreditation, is the daiamid epoxy curing agent of 650 as adopted purchased from Shanghai Resin Factory Co., Ltd.'s trade mark.
Part A before use, at room temperature mixes with part B by cold mixing epoxy bitumen material provided by the invention, obtains cold mixing epoxy bitumen material and be directly layed in road surface after stirring; Also the cold mixing epoxy bitumen material obtained at room temperature can be joined building stones with collection to mix, be layed in road surface.In the present invention, building stones gathering materials as AC-10 is joined in described integrating, and the AC-10 preferably utilizing basalt to prepare gathers materials.Described epoxy bitumen material and collection join the weight ratio of the bitumen aggregate ratio of building stones for (6.5 ~ 8): 100, are preferably (6.8 ~ 7.5): 100, are more preferably (6.8 ~ 7.2): 100.
The cold mixing epoxy bitumen material that the present invention obtains also can be used for pavement seam filling and repairs, and also can arterial street, Bus stand and airport pavement to lay and motorway and bridge etc. require higher occasion.
Experimental result shows, the average tensile strength of epoxy bitumen material provided by the invention is 1.87MPa, and elongation at break is 260%, and Marshall stability on average can reach 58KN, and dynamic stability is more above 13000 times/mm, shows as very excellent anti-rut behavior; After material places 24h under the condition of-20 DEG C, during splitting, material presents ductile rupture, shows this material high cold resistance energy.Stripping strength mean value is 43MPa, can have good cementability with basic foundation.
As well known to those skilled in the art, conventional modifying asphalt and epoxy bitumen material are when construction application, must first carry out after high temperature (150 ~ 180 DEG C) mixes and stirs under special batching plant, utilizing special asphalt thermal insulation car (120 DEG C) to be transported to working-yard, there is material and mixes and stirs the shortcomings such as energy consumption is high, transport difficulty is large in technology.Described part A is mixed 0.2 ~ 1h with part B by the present invention under room temperature (20 DEG C), obtains epoxy bitumen material, and the weight ratio of described part A and described part B is (7 ~ 12): 1.In epoxy bitumen material provided by the invention, part A mixes under room temperature (20 DEG C) with part B, epoxy bitumen material can be obtained, compared with prior art, epoxy bitumen material provided by the invention uses and heat insulation transportation without the need to carrying out heating, after part A and part B at room temperature mix, namely there is lower viscosity, mobility necessary when can ensure to construct.Reduce the energy consumption that epoxy bitumen material uses, when can effectively avoid heating, bitumen flue gas is to the damage of operator's health simultaneously, really achieves the requirement of energy-saving and environment friendly.In the present invention, consistent described in the weight ratio of the kind of described epoxy resin, part A and part B and technique scheme, does not repeat them here.
The invention has the beneficial effects as follows: the compatibility problem between the soluble matrix pitch of bituminous epoxy expanding material that the method obtains and epoxy resin, and the good mechanical property of bituminous epoxy (well having taken into account intensity and this two large index of toughness) can be given, the application of this bituminous epoxy expanding material at room temperature can be uniformly mixed, construct, effectively can overcome the restriction by season, weather, temperature in construction application process of conventional hot asphalt, can reduce Energy Consumption of Construction simultaneously, simplify difficulty of construction, the energy-conservation green realizing road and bridge face is mated formation.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the bituminous epoxy expanding material that the embodiment of the present invention 1 obtains.
Fig. 2 is the fluorescence micrograph of the epoxy bitumen material that the embodiment of the present invention 1 obtains.
Fig. 3 is the fluorescence micrograph of the epoxy bitumen material that the embodiment of the present invention 2 obtains.
Fig. 4 is the fluorescence micrograph of the epoxy bitumen material that the embodiment of the present invention 3 obtains.
Fig. 5 is the fluorescence micrograph of the epoxy bitumen material that the embodiment of the present invention 4 obtains.
Fig. 6 is the fluorescence micrograph of the epoxy bitumen material that the embodiment of the present invention 5 obtains.
Embodiment
The invention provides a kind of preparation method of bituminous epoxy expanding material, comprise the following steps:
A) heavy aromatics oil is heated to 60 ~ 180 DEG C;
B) mixed solution of a certain proportion of isocyanic ester, initiator and anti degradant is joined in heavy aromatics oil, under the condition of heating, stir 0.5 ~ 2h, bituminous epoxy expanding material can be obtained.
Preferably, in described heavy aromatics oil, heavy aromatics content is 30 ~ 85% (quality), is more preferably 50 ~ 80%, is more preferably 60 ~ 75%.
Preferably, the Heating temperature of described heavy aromatics oil is 60 ~ 180 DEG C, is more preferably 80 ~ 160 DEG C, is more preferably 120 ~ 150 DEG C.
Preferably, the consumption of described isocyanic ester is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, is more preferably 5 ~ 9%, is more preferably 6 ~ 8%.
Preferably, the consumption of described DHBP is attached most importance to 0.5 ~ 5% of aromatic hydrocarbon oil parts by weight, is more preferably 1 ~ 4%, is more preferably 1 ~ 3%.
Preferably, the consumption of described St is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, is more preferably 5 ~ 9%, is more preferably 6 ~ 8%.
Invention also provides a kind of using method of bituminous epoxy expanding material, comprise the following steps:
I) pitch is joined in common reactor be uniformly mixed with bituminous epoxy expanding material, bituminous epoxy thinner, epoxy resin together with epoxide diluent, obtain the part A of epoxy bitumen material;
Described part A comprises the component of following weight part:
II) by described step I) the epoxy bitumen material part A that obtains mixes with epoxy bitumen material part B agitating, obtain a kind of can the epoxy bitumen material of at room temperature construction usage;
Described part B comprises the component of following weight part:
20 ~ 50 parts, bituminous epoxy solidifying agent;
Described step I) and described step II) without sequencing.
III) by described step II) epoxy bitumen material that obtains directly is layed in road surface, or join after building stones mix with collection and be layed in road surface.
Preferably, described step I) agitating mixing time be 0.5 ~ 2h, step II) in agitating mixing time be 0.2 ~ 1h.
Preferably, described step I) agitating mixing temperature be room temperature ~ 180 DEG C independently of one another, step II) in agitating mixing temperature be room temperature.
Preferably, described step III) integrate and join building stones gathering materials as AC-10, the AC-10 preferably utilizing basalt to prepare gathers materials.
Preferably, described step III) epoxy bitumen material join the weight ratio of the bitumen aggregate ratio that building stones mixs for (6.5 ~ 8) with collection: 100, preferably (6.8 ~ 7.5): 100, be more preferably (6.8 ~ 7.2): 100.
The invention provides the using method of the epoxy bitumen material that method obtains described in epoxy bitumen material described in a kind of technique scheme and technique scheme, comprise the following steps:
Described epoxy bitumen material part A is mixed with epoxy bitumen material part B agitating, can obtain a kind of can the epoxy bitumen material of at room temperature construction usage;
Described epoxy bitumen material is directly layed in road surface, or joins after building stones mix with collection and be layed in road surface;
Preferably, building stones gathering materials as AC-10 is joined in integrating of described step, and the AC-10 preferably utilizing basalt to prepare gathers materials.
Preferably, epoxy bitumen material and the collection of described step join the weight ratio of the bitumen aggregate ratio that building stones mix for (6.5 ~ 8): 100, are preferably (6.8 ~ 7.5): 100, are more preferably (6.8 ~ 7.2): 100.
In the present invention, the step being mixed into other materials of those skilled in the art's accreditation do not mentioned in some above-mentioned steps can be inserted.The kind of the material be mixed into and add-on do not have special restriction, adopt the material of those skilled in the art's accreditation.
The present invention detects the performance of the epoxy bitumen material obtained, and detailed process is as follows:
The fluorescence micrograph shooting of epoxy bitumen material, stir after prepared bituminous epoxy A, B two portions are mixed in proportion, leave standstill 10min, getting supernatant liquid is applied on slide glass, cooling after coagulation film forming, under ultrasonic wave with washed with de-ionized water at least 30min with dispel surface impurity, utilize Nikon TE2000-U type fluorescence microscopy take fluorescence photo.For epoxy resin and pitch co-mixing system, occur at the rare fluorescence be excited of blue light section pitch, and epoxy resin obviously has yellow-green fluorescence to be excited out, epoxy resin phase (yellow-green colour) and pitch phase (black) clearly can be told under blue filter group is as the fluorescent microscope of exciting light, owing to being reflection light field, the form of polymkeric substance in pitch can not be destroyed, thus can observe truly epoxy resin pitch mutually in real morphological structure.
Be that the method recorded in the national standard " mensuration the 3rd part of plastic tensile performance: thin mould the test conditions with thin slice " of GBT 1040.3-2006 detects the tensile strength of the epoxy bitumen material obtained and elongation at break according to standard No..
Be that the stripping strength of method to the epoxy bitumen material obtained recorded in the national standard " tackiness agent 180 degree of peeling strength test method flexible materials are to rigid material " of GB/T 2790-1995 detects according to standard No..
Be the operable time of the epoxy bitumen material that the method test recorded in the industry standard " highway engineering pitch and Asphalt Mixture Experiment code " of JTJ052-2000 obtains, thermoset, Marshall stability, dynamic stability, freeze-thaw split strength ratio, anti-stretch bending strength, bending-type panel and maximum flexural-tensile strain according to standard No..
In order to further illustrate the present invention, below in conjunction with embodiment, epoxy bitumen material provided by the invention and preparation method thereof and using method are described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
Heavy aromatics oil (is protected magnificent petrochemical industry novel material exploitation limited-liability company purchased from Wuhan, down together) 100g is placed in the three-necked bottle of belt stirrer, after being heated to 150 DEG C with oil bath, after constant temperature 15min, slowly add 3-sec.-propyl-α, α-dimethylbenzyl isocyanic ester (TMI) is (purchased from ALDRICH company, lower same) 7.5g, vinylbenzene (St) is (purchased from Chemical Reagent Co., Ltd., Sinopharm Group, lower same) 7.5g and 2, 5-dimethyl-2, 5-bis(t-butylperoxy) hexane (DHBP) 2g is (purchased from Chengdu Li Jingxiwang Fine Chemical Co., Ltd, lower same), after stirring 1h, cooling, bituminous epoxy expanding material of the present invention can be obtained.The infrared spectrogram of the bituminous epoxy expanding material of Fig. 1 prepared by the present embodiment.
(trade mark is the shell pitch of No. 70 accurately to take 30g pitch, lower same), 12g bituminous epoxy expanding material, 10g bituminous epoxy thinner vinylbenzene is (purchased from Chemical Reagent Co., Ltd., Sinopharm Group, lower same), 8g epoxy resin diluent 632 is (purchased from Yu Sheng Chemical Co., Ltd. of Yantai City, lower same), (trade mark is E-51 to 20g epoxy resin, purchased from Ba Ling petrochemical industry limited liability company of SINOPEC, lower same), join in the common response still of 80 DEG C and stir 30min, obtain the part A of epoxy bitumen material.
By the part A of epoxy bitumen material and 10g epoxy hardener polyamide 6 50 (purchased from Shanghai Resin Factory Co., Ltd., down together) part B of epoxy bitumen material joins in normal-temperature reaction still and stirs 20min, after mixing, the mixture obtained is cooled to room temperature, obtains epoxy bitumen material.The fluorescence micrograph of the epoxy bitumen material of Fig. 2 prepared by the present embodiment.
By the epoxy bitumen material obtained by above-mentioned steps, be the part by weight of 100:7 by bitumen aggregate ratio, add gathering materials of AC-10, stir 60s in SYD-F02-20 automatic coagulation conjunction material amalgamator after, marshal piece is prepared by T0702 typical compacting method, two-sided respectively hit real 50 times after, after product completion of cure, epoxy asphalt concrete material of the present invention can be prepared into.
Epoxy bitumen material obtained by the present invention and epoxy asphalt concrete material carry out performance test, and test result is as shown in table 1.
Table 1 bituminous epoxy and epoxy asphalt concrete the performance test results
As can be seen from Table 1, tensile strength mean value after epoxy bitumen material solidification is 1.87Pa, tension set mean value is 260%, all considerably beyond U.S. bituminous epoxy technical indicator (tensile strength >=1.5Mpa, tension set >=200%) requirement, prove that this kind of material has well taken into account intensity and this two large index of toughness.
The bituminous concrete that epoxy bitumen material provided by the invention and building stones are mixed to get Marshall stability of compound after health reaches 58KN, embody superior elasticity and the bonding capacity of this epoxy bitumen material, reflect the excellent the mechanical properties and performance of this kind of epoxy asphalt mixture from the side.
Epoxy asphalt mixture of the present invention is after freeze-thaw cycle, and freeze-thaw split intensity, on average up to 86%, exceedes 75% required by technical indicator, and what this material was described has comparatively excellent water stabilizing.
After dynamic stability test under 80 DEG C of conditions completes, dynamic stability reaches 13000 times/more than mm.Excellent rutting resistance embodies the outstanding high temperature stability performance of epoxy asphalt mixture that the present invention obtains, can meet the pavement performance under the steel box girder bridge face high temperature of 70 DEG C in summer very well, occur rut disease under avoiding high temperature.
What low-temperature bending test was dry straight meets technical indicator, embodies epoxy asphalt mixture that the present invention obtains while possessing high strength, also has good low-temperature cracking-resistance.The snappiness of its low temperature is very great for the feature meaning meeting steel box girder bridge facial disfigurement larger.
Embodiment 2
Heavy aromatics oil 100g is placed in the three-necked bottle of belt stirrer, after being heated to 60 DEG C with oil bath, after constant temperature 15min, slowly add 3-sec.-propyl-alpha, alpha-dimethylbenzyl isocyanic ester (TMI) 3g, vinylbenzene (St) 3g and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DHBP) 0.5g, after stirring 1h, cooling, can obtain bituminous epoxy expanding material of the present invention.
Accurately take 30g pitch, 10g bituminous epoxy expanding material, 5g bituminous epoxy thinner vinylbenzene, 5g epoxy resin diluent 632,20g epoxy resin, joins in the common reactor of 80 DEG C and stirs 30min, obtain the part A of epoxy bitumen material.
By the part A of epoxy bitumen material and 5g epoxy hardener polyamide 6 50, the part B of epoxy bitumen material joins in normal-temperature reaction still and stirs 20min, after mixing, the mixture obtained is cooled to room temperature, obtains epoxy bitumen material.The fluorescence micrograph of the epoxy bitumen material of Fig. 3 prepared by the present embodiment.By the epoxy bitumen material obtained by above-mentioned steps, be the part by weight of 100:7 by bitumen aggregate ratio, add gathering materials of AC-10, stir 60s in SYD-F02-20 automatic coagulation conjunction material amalgamator after, marshal piece is prepared by T0702 typical compacting method, two-sided respectively hit real 50 times after, after product completion of cure, epoxy asphalt concrete material of the present invention can be prepared into.
Epoxy bitumen material obtained by the present invention and epoxy asphalt concrete material carry out performance test, and test result is as shown in table 2.
Table 2 bituminous epoxy and epoxy asphalt concrete the performance test results
Embodiment 3
Heavy aromatics oil 100g is placed in the three-necked bottle of belt stirrer, after being heated to 160 DEG C with oil bath, after constant temperature 15min, slowly add 3-sec.-propyl-alpha, alpha-dimethylbenzyl isocyanic ester (TMI) 10g, vinylbenzene (St) 10g and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DHBP) 5g (, after stirring 1h, cooling, can obtain bituminous epoxy expanding material of the present invention.
Accurately take 30g pitch, 15g bituminous epoxy expanding material, 15g bituminous epoxy thinner vinylbenzene, 15g epoxy resin diluent 632,30g epoxy resin, joins in the common response still of 80 DEG C and stirs 30min, obtain the part A of epoxy bitumen material.
The part B of the part A of epoxy bitumen material and 15g epoxy hardener polyamide 6 50 epoxy bitumen material is joined in normal-temperature reaction still and stirs 20min, after mixing, the mixture obtained is cooled to room temperature, obtains epoxy bitumen material.The fluorescence micrograph of the epoxy bitumen material of Fig. 4 prepared by the present embodiment.
By the epoxy bitumen material obtained by above-mentioned steps, be the part by weight of 100:7 by bitumen aggregate ratio, add gathering materials of AC-10, stir 60s in SYD-F02-20 automatic coagulation conjunction material amalgamator after, marshal piece is prepared by T0702 typical compacting method, two-sided respectively hit real 50 times after, after product completion of cure, epoxy asphalt concrete material of the present invention can be prepared into.
Epoxy bitumen material obtained by the present invention and epoxy asphalt concrete material carry out performance test, and test result is as shown in table 3.
Table 3 bituminous epoxy and epoxy asphalt concrete the performance test results
Embodiment 4
Heavy aromatics oil 100g is placed in the three-necked bottle of belt stirrer, after being heated to 140 DEG C with oil bath, after constant temperature 15min, slowly add 3-sec.-propyl-alpha, alpha-dimethylbenzyl isocyanic ester (TMI) 7g, vinylbenzene (St) 7g and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DHBP) 1.8g, after stirring 1h, cooling, can obtain bituminous epoxy expanding material of the present invention.
Accurately take 30g pitch, 14g bituminous epoxy expanding material, 9g bituminous epoxy thinner vinylbenzene, 9g epoxy resin diluent 632,20g epoxy resin joins in the common response still of 80 DEG C and stirs 30min, obtains the part A of epoxy bitumen material.
By the part A of epoxy bitumen material and 10g epoxy hardener polyamide 6 50, the part B of epoxy bitumen material joins in normal-temperature reaction still and stirs 20min, after mixing, the mixture obtained is cooled to room temperature, obtains epoxy bitumen material.The fluorescence micrograph of the epoxy bitumen material of Fig. 5 prepared by the present embodiment.
By the epoxy bitumen material obtained by above-mentioned steps, be the part by weight of 100:7.2 by bitumen aggregate ratio, add gathering materials of AC-10, stir 60s in SYD-F02-20 automatic coagulation conjunction material amalgamator after, marshal piece is prepared by T0702 typical compacting method, two-sided respectively hit real 50 times after, after product completion of cure, epoxy asphalt concrete material of the present invention can be prepared into.
Epoxy bitumen material obtained by the present invention and epoxy asphalt concrete material carry out performance test, and test result is as shown in table 4.
Table 4 bituminous epoxy and epoxy asphalt concrete the performance test results
Embodiment 5
Heavy aromatics oil 100g is placed in the three-necked bottle of belt stirrer, after being heated to 160 DEG C with oil bath, after constant temperature 15min, slowly add 3-sec.-propyl-alpha, alpha-dimethylbenzyl isocyanic ester (TMI) 7g, vinylbenzene (St) 7g and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DHBP) 1.8g, after stirring 1h, cooling, can obtain bituminous epoxy expanding material of the present invention.
Accurately take 30g pitch, 14g bituminous epoxy expanding material, 10g bituminous epoxy thinner vinylbenzene, 10g epoxy resin diluent 632,20g epoxy resin, joins in the common response still of 80 DEG C and stirs 30min, obtain the part A of epoxy bitumen material.
The part B of the part A of epoxy bitumen material and 14g epoxy hardener polyamide 6 50 epoxy bitumen material is joined in normal-temperature reaction still and stirs 20min, after mixing, the mixture obtained is cooled to room temperature, obtains epoxy bitumen material.The fluorescence micrograph of the epoxy bitumen material of Fig. 6 prepared by the present embodiment.
By the epoxy bitumen material obtained by above-mentioned steps, be the part by weight of 100:7.2 by bitumen aggregate ratio, add gathering materials of AC-10, stir 60s in SYD-F02-20 automatic coagulation conjunction material amalgamator after, marshal piece is prepared by T0702 typical compacting method, two-sided respectively hit real 50 times after, after product completion of cure, epoxy asphalt concrete material of the present invention can be prepared into.
Epoxy bitumen material obtained by the present invention and epoxy asphalt concrete material carry out performance test, and test result is as shown in table 5.
Table 5 bituminous epoxy and epoxy asphalt concrete the performance test results
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for bituminous epoxy expanding material, is characterized in that comprising the following steps:
A) heavy aromatics oil is heated to 60 ~ 180 DEG C;
B) to attach most importance to by the consumption of isocyanic ester 3 ~ 10% of aromatic hydrocarbon oil parts by weight, the consumption of initiator is attached most importance to 0.5 ~ 5% of aromatic hydrocarbon oil parts by weight, the consumption of anti degradant is attached most importance to 3 ~ 10% of aromatic hydrocarbon oil parts by weight, isocyanic ester, initiator and anti degradant are joined in heavy aromatics oil, under the condition of heating, stir 0.5 ~ 2h, obtain bituminous epoxy expanding material.
2. the preparation method of a kind of bituminous epoxy expanding material according to claim 1, is characterized in that, in described heavy aromatics oil, heavy aromatics content is 30 ~ 85%, is preferably 50 ~ 80%, is more preferably 60 ~ 75%;
The Heating temperature of described heavy aromatics oil is 60 ~ 180 DEG C, is preferably 80 ~ 160 DEG C, is more preferably 120 ~ 150 DEG C.
3. the preparation method of a kind of bituminous epoxy expanding material according to claim 1, is characterized in that, the consumption of described isocyanic ester is attached most importance to 5 ~ 9% of aromatic hydrocarbon oil parts by weight, is preferably 6 ~ 8%;
Described isocyanic ester can be at least one in tolylene diisocyanate, '-diphenylmethane diisocyanate, poly methylene poly phenyl poly isocyanate.
4. the preparation method of a kind of bituminous epoxy expanding material according to claim 1, it is characterized in that, described initiator is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, consumption is attached most importance to 0.5 ~ 5% of aromatic hydrocarbon oil parts by weight, is preferably 1 ~ 4%, is more preferably 1 ~ 3%.
5. the preparation method of a kind of bituminous epoxy expanding material according to claim 1, is characterized in that, described anti degradant is vinylbenzene, and consumption is attached most importance to 5 ~ 9% of aromatic hydrocarbon oil parts by weight, is more preferably 6 ~ 8%.
6. as claim 1 a kind of application of bituminous epoxy expanding material that obtains, it is characterized in that comprising the following steps:
1) pitch, bituminous epoxy expanding material, bituminous epoxy thinner, epoxy resin, epoxy resin diluent are joined in reactor together and be uniformly mixed, obtain the part A of epoxy bitumen material;
Described part A comprises the component of following weight part:
2) by described step 1) part A of epoxy bitumen material that obtains mixes with the part B agitating of epoxy bitumen material, obtain a kind of can the epoxy bitumen material of at room temperature construction usage.
Described part B comprises the component of following weight part:
20 ~ 50 parts, bituminous epoxy solidifying agent;
3) by step 2) described epoxy bitumen material is directly layed in road surface, or join after building stones mix with collection and be layed in road surface.
Described step 3) integrate and join building stones gathering materials as AC-10, the AC-10 preferably utilizing basalt to prepare gathers materials.
Described epoxy bitumen material and collection join the weight ratio of the bitumen aggregate ratio of building stones for (6.5 ~ 8): 100, are preferably (6.8 ~ 7.5): 100, are more preferably (6.8 ~ 7.2): 100.
7. the application of a kind of bituminous epoxy expanding material according to claim 6, is characterized in that, described pitch is at least one in petroleum pitch, oxidized bitumen, coal-tar pitch, lake pitch, multiple by any proportioning mixing.
8. the application of a kind of bituminous epoxy expanding material according to claim 6, is characterized in that, described step 1) agitating mixing time be 0.5 ~ 2h;
Described step 1) agitating mixing temperature be room temperature ~ 180 DEG C, step 2) in agitating mixing temperature be room temperature.
9. the application of a kind of bituminous epoxy expanding material according to claim 6, is characterized in that, the weight part of bituminous epoxy expanding material is 15 ~ 45 parts, is preferably 20 ~ 40 parts;
The weight part of the bituminous epoxy thinner of part A is 10 ~ 45 parts, is preferably 20 ~ 40 parts;
The bituminous epoxy thinner of described part A is at least one in vinylbenzene, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, multiple by any proportioning mixing;
Described epoxy resin is at least one in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, dihydroxyphenyl propane D type epoxy resin, resorcinol type epoxy, multiple by any proportioning mixing.
The weight part of the epoxy resin diluent of described part A is 10 ~ 45 parts, is preferably 20 ~ 40 parts;
Described epoxy resin diluent is styrene oxide, phenyl glycidyl ether, p-cresol glycidyl ether, 2-Racemic glycidol phenyl glycidyl ether, 2, at least one in 6-2-glycidyl phenyl glycidyl ether, o-phthalic acid diglycidyl ester, tetrahydrophthalic acid 2-glycidyl ester, hexahydrophthalic acid 2-glycidyl ester, multiple by any proportioning mixing.
10. the application of a kind of bituminous epoxy expanding material according to claim 6, is characterized in that, the weight part of the bituminous epoxy solidifying agent of part B is 20 ~ 50 parts, is preferably 20 ~ 40 parts, is more preferably 20 ~ 35 parts;
Described bituminous epoxy solidifying agent is at least one in fatty amines solidifying agent, alicyclic ring amine curing agent, aromatic amine curing agent, polyamide-based solidifying agent, multiple by any proportioning mixing.
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| CN117624919A (en) * | 2023-11-20 | 2024-03-01 | 北京建筑大学 | Cold-mixing cold-paving vegetable oil-based epoxy asphalt and preparation method thereof |
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