CN107151419B - A kind of high tenacity cold mixing bituminous epoxy binder and preparation method thereof - Google Patents
A kind of high tenacity cold mixing bituminous epoxy binder and preparation method thereof Download PDFInfo
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- CN107151419B CN107151419B CN201710540037.7A CN201710540037A CN107151419B CN 107151419 B CN107151419 B CN 107151419B CN 201710540037 A CN201710540037 A CN 201710540037A CN 107151419 B CN107151419 B CN 107151419B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/44—Amides
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Road Paving Structures (AREA)
Abstract
The present invention provides a kind of high tenacity cold mixing bituminous epoxy binder and preparation method thereof.Cold mixing bituminous epoxy binder includes component A and component B, and component A is mainly made of epoxy resin, diluent and toughener, and component B is mainly made of curing agent, pitch, diluent, compatilizer and defoaming agent.Cold mixing bituminous epoxy binder of the invention can be mixed and stirred and be constructed under room temperature, low-carbon environment-friendly and construction technology is simple.3 D stereo network structure is formed after epoxy bitumen material solidification, there is good thermal stability and adhesion strength.It uses branching nbr carboxyl terminal for toughener, guarantees the excellent flexibility of bituminous epoxy solidfied material.The present invention is mainly suitable for the bonding on the road surfaces such as Steel Bridge Deck, urban viaduct, cement concrete bridge deck, tunnel, highway and waterproofs.
Description
Technical field
The present invention relates to road and bridge construction materials and preparation method thereof, and in particular to a kind of high tenacity cold mixing epoxy drip
Green binder material and preparation method thereof.
Background technique
During deck paving, setting water-proof tack coat be to ensure that deck installation structure durability important measures it
One.During deck paving, moisture penetrates into bridge floor in order to prevent, and reinforcing bar or steel bridge deck in corrosion concrete threaten bridge
Floorings and pave-load layer are bonded to an entirety by safety beam, water-proof tack coat of mating formation, and not only improve floorings and pave-load layer
Stress condition, additionally it is possible to prevent moisture from penetrating into.
Material for paving steel bridge deck adhesive layer mainly has heat molten type binding material, solvent type binding material and thermosetting property
Binding material.Heat molten type binding material adds resin (such as rosin) and various high molecular materials (such as ethylene-acetate second by pitch
Alkene (vinyl acetate) ester copolymer, polyethylene and butadiene-styrene rubber etc.) composition.Heat molten type binding material has certain deformation energy
Power has follow-up capability to steel plate deformed, it may have good waterproof action.However, such material is easy to soften at high temperature,
Cohesive force decline.Moreover, heat molten type material must sufficiently melt before construction, stirred evenly after being warming up to defined temperature, then
It is uniformly dispensed with pitch truck spreader, difficulty of construction is relatively large.Preheating before construction can also reduce the viscous of heat molten type binding material
Tie effect.Solvent type binding material generally refers to emulsified asphalt and soluble rubber asphalt more, the disadvantage is that high temperature easily softens, and material
Material is internal to contain heat-sensitive substance, and gas can be released when paving high temperature by meeting, so that pave-load layer be made to generate bubble.
Thermoset binder material refers to bituminous epoxy.Bituminous epoxy is a kind of with thermosetting epoxy resin modified asphalt material,
So that thermoplastic pitch is fundamentally changed into thermosetting material, assigns the excellent mechanical strength of bituminous epoxy, flexibility, resistance to tired
The features such as labor performance, high temperature resistance and corrosion resistance.No matter bituminous epoxy is in cohesive force, deformability or in heat
In terms of stability, all there is significant advantage.Epoxy bitumen material is expensive, and especially import bituminous epoxy price is usually in 5-
60000 yuan/ton.Moreover, thermosetting epoxy asphalt complicated construction technique, needs to use special sprinkling for (190 DEG C or so) at high temperature
Equipment is constructed.Therefore, it is necessary to develop can in room temperature mix and stir the bituminous epoxy binder of construction for road and bridge waterproof with
Bonding.
Summary of the invention
It is an object of the invention to propose a kind of high tenacity cold mixing bituminous epoxy binder and preparation method thereof, the cold mixing ring
Oxygen asphalt material have the characteristics that excellent adhesive property, mechanical strength, flexibility, can room temperature to mix and stir construction, curing time short,
Bridge deck water-proof tack coat is primarily adapted for use in mat formation.
The invention proposes a kind of high tenacity cold mixing bituminous epoxy binders, including component A and component B, component A include ring
Oxygen resin, diluent and toughener, component B include curing agent, pitch, diluent, compatilizer and defoaming agent.
Each component parts by weight in component A are as follows:
100 parts of epoxy resin
5-20 parts of toughener
10-30 parts of diluent
Each component parts by weight in component B are as follows:
Wherein, the mass ratio of component A and component B are 100:110-100:200.
Preferably, the epoxy resin is liquid bisphenol A type tetraglycidel ether epoxy resin.
Preferably, the toughener is branching nbr carboxyl terminal (b-CTBN), and structural formula is as follows:
Preferably, the curing agent is low molecular polyamides, and structural formula is as follows:
Preferably, the pitch is SBS modified pitch.
Preferably, the component B diluent be pitch good solvent, including acetone, toluene, dimethylbenzene, dichloropropane,
The mixture of one or more of tetrachloro-ethylene, dibutyl phthalate, dioctyl phthalate.
Preferably, the compatilizer is big for stearic acid or stearate containing epoxy group and fatty long-chain, including epoxy
Soya-bean oil, epoxystearic acid, epoxy stearate, epoxyoleic acid, Epoxy oil acid esters, epoxy linoleic acid, epoxy linoleate and poly-
The mixture of one or more of ethylene oxide stearic acid.
Preferably, the defoaming agent is polysiloxane defoaming agent.
The invention also discloses a kind of methods for preparing above-mentioned high tenacity cold mixing bituminous epoxy binder, including following step
It is rapid:
The preparation of component A: by epoxy resin, diluent and toughener mix, be heated to 40-60 DEG C, with 200-500 turn/
The rate of minute stirs 1-6 hours, is cooled to room temperature to obtain the component A of high tenacity cold mixing bituminous epoxy binder.
The preparation of component B: pitch is heated to 110-135 DEG C of melting.It weighs pitch and diluent and mixes, with 200-
500 revs/min of rate is stirred 0.5-2 hours and is completely dissolved to pitch.40 DEG C are cooled to hereinafter, curing agent, compatilizer is added
And defoaming agent, it is stirred 1-4 hours with 200-500 revs/min of rate, obtains the component of high tenacity cold mixing bituminous epoxy binder
B。
A kind of concrete application method of high tenacity cold mixing bituminous epoxy binder, it is to mix component A and component B in room temperature
It closes, is stirred rapidly 3-5 minutes with 500~900 revs/min of rate, obtain the mixture of high tenacity cold mixing bituminous epoxy.
Preferably, in component A toughener the preparation method comprises the following steps: using trimethylolpropane as core, by carboxyl end group butyronitrile rubber
Glue, trimethylolpropane, catalyst and hexamethylene mixing, wherein the molar ratio of trimethylolpropane and nbr carboxyl terminal is
3:4 back flow reaction 1-8 hours, passes through vacuum distillation removing solvent after reaction.It is washed using ether and passes through Soxhlet extraction
Residual solvent, small molecule by-product and unreacted monomer are removed, extract is finally placed in vacuum drying oven drying, obtains b-
CTBN。
Beneficial effect caused by the present invention includes:
(1) construction technology is simple, using low molecular polyamides as curing agent, can mix and stir construction, energy conservation and environmental protection at normal temperature；
(2) good mechanical performance is guaranteeing epoxy bitumen material intensity using the nitrile rubber flexibilizing epoxy pitch of branching
On the basis of significantly improve the flexibility of epoxy bitumen material；
(3) applied widely, it is applicable not only to Steel Bridge Deck water-proof tack coat and mats formation, it may also be used for urban viaduct, cement
The bonding and waterproof on the road surfaces such as concrete bridge deck, tunnel, highway.
Specific embodiment
The present invention is further illustrated with example below, but protection scope of the present invention is not limited in examples of implementation.To this
The other changes and modifications that the technical staff in field makes in the case of without departing from the spirit and scope of protection of the present invention
Including within that scope of the present invention.
Toughener b-CTBN's the preparation method is as follows:
Embodiment 1:
Using trimethylolpropane as core, by nbr carboxyl terminal, trimethylolpropane, catalyst for esterification reaction and molten
The mixing of agent hexamethylene, wherein the molar ratio of trimethylolpropane and nbr carboxyl terminal is 3:4, and catalyst amount is end ring oxygen
The 1% of base nitrile rubber and trimethylolpropane quality sum, the quality of hexamethylene are nbr carboxyl terminal and trihydroxy methyl
10 times of propane quality sum, back flow reaction 3h, passes through vacuum distillation removing hexamethylene after reaction under mechanical stirring.It is cold
But it is washed 3 times to after room temperature using ether, by sediment by Soxhlet extraction for 24 hours to remove remaining solvent, small molecule by-product
Object and unreacted monomer.Extract is placed in vacuum drying oven drying, obtains b-CTBN.
High tenacity cold mixing bituminous epoxy binder the preparation method is as follows:
Embodiment 2:
Weigh 100 parts of (mass parts, similarly hereinafter) liquid bisphenol A type tetraglycidel ether epoxy resins (E51), 5 parts of b-CTBN, 15
Part octyl glycidyl ether, is heated to 40 DEG C, is stirred 2 hours with 300 revs/min of rate, is cooled to room temperature, obtains high tenacity
The component A of cold mixing bituminous epoxy binder.
SBS modified pitch is placed in convection oven, in 110 DEG C heating melting 2 hours.Weigh 90 parts of SBS modified pitch
With 35 parts of dichloropropanes, stirred 2 hours with 300 revs/min of rate.40 DEG C are cooled to gather hereinafter, 100 parts of low molecular weights are added
Amide, 30 parts of epoxystearic acids and 1 part of polysiloxanes are stirred 1 hour with 300 revs/min of rate, obtain high tenacity cold mixing ring
The component B of oxygen pitch binder.
100 parts of component A and 150 parts of component B are mixed at room temperature, is stirred 5 minutes, is obtained with 800 revs/min of rate
The mixture of high tenacity cold mixing bituminous epoxy binder.Said mixture is taken to pour into Teflon mould, normal temperature cure 36
Hour, cold mixing bituminous epoxy solidfied material dumbbell shape sample is obtained after demoulding, is used for Mechanics Performance Testing.Mechanics Performance Testing condition
It is 23 ± 2 DEG C, rate of extension 10mm/min.Adhesion strength is tested using drawing instrument.It stretches and pull-out test result is seen attached list
1。
Embodiment 3:
100 parts of E51,12 parts of b-CTBN and 10 part of butyl glycidyl ethers are weighed, 60 DEG C are heated to, with 300 revs/min
Rate stirs 2 hours, is cooled to room temperature, obtains the component A of high tenacity cold mixing bituminous epoxy binder.
SBS modified pitch is placed in convection oven, in 120 DEG C heating melting 1.5 hours.Weigh the modified drip of 60 parts of SBS
Green and 25 parts of dioctyl phthalates are stirred 2 hours with 200 revs/min of rate.40 DEG C are cooled to hereinafter, being added 100 parts
Low molecular polyamides, 15 parts of epoxidized soybean oils and 0.5 part of polysiloxanes are stirred 1 hour with 500 revs/min of rate, are obtained
The component B of high tenacity cold mixing bituminous epoxy binder.
100 parts of component A and 200 parts of component B are mixed at room temperature, is stirred 5 minutes, is obtained with 500 revs/min of rate
The mixture of high tenacity cold mixing bituminous epoxy binder.Said mixture is taken to pour into Teflon mould, normal temperature cure 24
Hour, cold mixing bituminous epoxy solidfied material dumbbell shape sample is obtained after demoulding, is used for Mechanics Performance Testing.Mechanics Performance Testing condition
It is 23 ± 2 DEG C, rate of extension 10mm/min.Adhesion strength is tested using drawing instrument.It stretches and pull-out test result is seen attached list
1。
Embodiment 4:
Weigh 100 parts of E51,20 parts of b-CTBN and 30 part of 12-14 alkyl glycidyl ethers, be heated to 50 DEG C, with 200 turns/
The rate of minute stirs 6 hours, is cooled to room temperature, obtains the component A of high tenacity cold mixing bituminous epoxy binder.
SBS modified pitch is placed in convection oven, in 135 DEG C heating melting 1 hour.Weigh 150 parts of SBS modified pitch
With 70 parts of dioctyl phthalates, stirred 0.5 hour with 500 revs/min of rate.40 DEG C are cooled to hereinafter, being added 100 parts
Low molecular polyamides, 55 parts of epoxy stearates and 2 parts of polysiloxanes are stirred 4 hours with 200 revs/min of rate, are obtained
The component B of high tenacity cold mixing bituminous epoxy binder.
100 parts of component A and 110 parts of component B are mixed at room temperature, is stirred 3 minutes, is obtained with 900 revs/min of rate
The mixture of high tenacity cold mixing bituminous epoxy binder.Said mixture is taken to pour into Teflon mould, normal temperature cure 24
Hour, cold mixing bituminous epoxy solidfied material dumbbell shape sample is obtained after demoulding, is tested for tensile property.Tensile property test condition
It is 23 ± 2 DEG C, rate of extension 10mm/min.Adhesion strength is tested using drawing instrument.It stretches and pull-out test result is seen attached list
1。
Embodiment 5:
100 parts of E51,10 parts of b-CTBN and 30 part of octyl glycidyl ethers are weighed, 40 DEG C are heated to, with 400 revs/min
Rate stirs 3 hours, is cooled to room temperature, obtains the component A of high tenacity cold mixing bituminous epoxy binder.
SBS modified pitch is placed in convection oven, in 120 DEG C heating melting 1.5 hours.Weigh the modified drip of 120 parts of SBS
Green and 50 parts of tetrachloro-ethylenes are stirred 2 hours with 300 revs/min of rate.40 DEG C are cooled to hereinafter, 100 parts of low molecular weights are added
Polyamide, 40 parts of Epoxy oil acid esters and 1.5 parts of polysiloxanes are stirred 2 hours with 300 revs/min of rate, it is cold to obtain high tenacity
The component B of mixed epoxy bitumen binder.
100 parts of component A and 120 parts of component B are mixed at room temperature, is stirred 3 minutes, is obtained with 900 revs/min of rate
The mixture of high tenacity cold mixing bituminous epoxy binder.Said mixture is taken to pour into Teflon mould, normal temperature cure 24
Hour, cold mixing bituminous epoxy solidfied material dumbbell shape sample is obtained after demoulding, is tested for tensile property.Tensile property test condition
It is 23 ± 2 DEG C, rate of extension 10mm/min.Adhesion strength is tested using drawing instrument.It stretches and pull-out test result is seen attached list
1。
The mechanical property of 1 high tenacity cold mixing bituminous epoxy binder of subordinate list
Claims (6)
1. a kind of high tenacity cold mixing bituminous epoxy binder, it is characterised in that: including component A and component B, the component A and group
The mass ratio for dividing B is 100:110-100:200；
The component A includes the substance of following parts by weight:
100 parts of epoxy resin；
5-20 parts of toughener；
10-30 parts of diluent；
The component B includes the substance of following parts by weight:
100 parts of curing agent；
60-150 parts of pitch；
25-70 parts of diluent；
15-55 parts of compatilizer；
0.5-2 parts of defoaming agent；
Curing agent in the component B is low molecular polyamides, and pitch is SBS modified pitch, the component in the component B
Toughener in A is branching nbr carboxyl terminal, and the toughener in the component A is made by following steps: a. is with three
Hydroxymethyl-propane is core, nbr carboxyl terminal, trimethylolpropane, catalyst and hexamethylene is mixed, wherein three hydroxyl first
The molar ratio of base propane and nbr carboxyl terminal carboxyl be 3:4, back flow reaction 1-8 hours；
B. it by vacuum distillation removing solvent, is washed using ether and residual solvent, small molecule by-product is removed by Soxhlet extraction
Object and unreacted monomer；
C. extract is placed in vacuum drying oven drying, obtains the toughener of high tenacity cold mixing bituminous epoxy binder.
2. high tenacity cold mixing bituminous epoxy binder according to claim 1, it is characterised in that: epoxy in the component A
Resin is liquid bisphenol A type tetraglycidel ether epoxy resin, and diluent is reactive epoxies diluent.
3. high tenacity cold mixing bituminous epoxy binder according to claim 1, it is characterised in that: diluent is the good of pitch
Solvent, compatilizer are stearic acid or stearate containing epoxy group and fatty long-chain, and defoaming agent is polysiloxane defoaming agent.
4. high tenacity cold mixing bituminous epoxy binder according to claim 1 or 3, it is characterised in that: the component B's is dilute
Releasing agent includes acetone, toluene, dimethylbenzene, dichloropropane, tetrachloro-ethylene, dibutyl phthalate, dioctyl phthalate
One or more of mixture.
5. high tenacity cold mixing bituminous epoxy binder according to claim 1, it is characterised in that: the component B's is compatible
Agent includes epoxidized soybean oil, epoxystearic acid, epoxy stearate, epoxyoleic acid, Epoxy oil acid esters, epoxy linoleic acid, epoxy
The mixture of one or more of linoleate and polyethylene oxide stearic acid.
6. a kind of preparation method for preparing high tenacity cold mixing bituminous epoxy binder described in claim 1, it is characterised in that:
The preparation of component A: epoxy resin, diluent and toughener are mixed in mass ratio, are heated to 40-60 DEG C, with 200-500
Rev/min rate stir 1-6 hours, be cooled to room temperature, obtain the component A of high tenacity cold mixing bituminous epoxy binder；
The preparation of component B: pitch is heated to 110-135 DEG C of melting, in mass ratio mix asphalt and diluent and stirring extremely drip
Blueness is completely dissolved, and simultaneously curing agent, compatilizer and defoaming agent is added in cooling, is stirred 1-4 hours with 200-500 revs/min of rate,
Obtain the B component of high tenacity cold mixing bituminous epoxy binder；
Component A is mixed with component B, is stirred rapidly 3-5 minutes and is made with 500-900 revs/min of rate；
Toughener in the component A is made by following steps: a. is using trimethylolpropane as core, by carboxyl end group butyronitrile
Rubber, trimethylolpropane, catalyst and hexamethylene mixing, wherein trimethylolpropane and nbr carboxyl terminal carboxyl rub
You than be 3:4, back flow reaction 1-8 hours；
B. it by vacuum distillation removing solvent, is washed using ether and residual solvent, small molecule by-product is removed by Soxhlet extraction
Object and unreacted monomer；
C. extract is placed in vacuum drying oven drying, obtains the toughener of high tenacity cold mixing bituminous epoxy binder.
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| CN108914737A (en) * | 2018-06-10 | 2018-11-30 | 重庆诚邦路面材料有限公司 | A kind of fine antiskid wearing layer of cement pavement EAP and construction method |
| CN109337297B (en) * | 2018-10-17 | 2021-02-02 | 河海大学 | High-asphalt-content cold-mix epoxy asphalt for road and bridge pavement and preparation method and application thereof |
| CN109797648B (en) * | 2019-03-21 | 2021-10-26 | 河南省交通规划设计研究院股份有限公司 | Waterproof bonding layer material for cement concrete bridge deck pavement |
| CN110372834A (en) * | 2019-07-31 | 2019-10-25 | 文山州广那高速公路投资建设开发有限公司 | Cold mixing type colour epoxy pitch, compatilizer and preparation method |
| CN113773800A (en) * | 2021-09-16 | 2021-12-10 | 南京朝科路桥工程技术有限公司 | Environment-friendly epoxy asphalt binder and preparation method thereof |
| 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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