CN107513277A

CN107513277A - Warm mixed epoxy bitumen, contain its compound and preparation method thereof

Info

Publication number: CN107513277A
Application number: CN201610433023.0A
Authority: CN
Inventors: 张静; 孙剑锋; 范思远; 张志银; 陈保莲; 宋乐春; 姚春雷; 宁爱民; 李志军; 程国香
Original assignee: China Petroleum and Chemical Corp; Sinopec Fushun Research Institute of Petroleum and Petrochemicals
Current assignee: China Petroleum and Chemical Corp; Sinopec Fushun Research Institute of Petroleum and Petrochemicals
Priority date: 2016-06-17
Filing date: 2016-06-17
Publication date: 2017-12-26

Abstract

The invention discloses a kind of warm mixed epoxy bitumen.The product includes warm-mixed asphalt, composition epoxy resin and curing agent；The warm-mixed asphalt includes warm-mixing agent and matrix pitch.Wherein warm-mixing agent preparation method is：Using F T synthetic products as raw material, hydro-conversion is carried out first；Hydrogenation products obtain the warm-mixing agent through sweating process again.Liquid composition is carried out using air-flow by material bed in sweating journey, strengthen solids fraction and the separating effect of liquid composition, while decomposed using inorganic salts and to produce gas in material bed middle formation short space, promote the quick outflow of liquid composition.The warm-mixing agent that uses can not only play warm mix effect to pitch in the warm mixed epoxy bitumen of the present invention, can also improve the heat endurance of pitch, improve thermal ageing resistant performance, reduce the melting temperature and viscosity at this temperature of pitch, reduce the generating capacity of pernicious gas.

Description

Warm mixed epoxy bitumen, contain its compound and preparation method thereof

Technical field

The present invention relates to a kind of pitch, and in particular to a kind of warm mixed epoxy bitumen and preparation method thereof.

Background technology

With being continuously increased for highway mileage, highway bridge quantity also increases therewith.Asked however, also exposing some Topic, wherein between bridge deck pavement and between pave-load layer and panel water-proof tack coat failure caused by disease account for it is larger Ratio, cause the attention in the industry to bridge deck pavement material and technique.As bridge floor interlaminar bonding material, by adding in pitch Add bituminous epoxy obtained from epoxy resin that there is preferable effect.However, because the viscosity of bituminous epoxy is larger, in construction It is required that construction temperature is higher, also there is certain operable time, so adding difficulty of construction；In addition, add in pitch After adding epoxy resin, pitch can be made to become fragile, pliability is deteriorated, bad with the followability of bridge panel.In order to solve these problems, Warm mix technology need to be taken, the construction temperature of bituminous epoxy is reduced and improves pliability.

Warm-mixed asphalt technology mainly has three kinds of modes：First, using the higher emulsified asphalt of evaporated residue content, 80 DEG C~120 DEG C at a temperature of it is low compared with the temperature of hot asphalt about 30 DEG C~50 DEG C with building stones mix, which；Second, mixed in mixing Water during material（Or the aqueous solution of surfactant）Added simultaneously in mix tank with pitch, due to the presence of water, make asphalt foaming, Reach viscosity reducing effect.But above two method can produce substantial amounts of vapor, easily cause equipment corrosion, stone also frequently occurs Powder conglomeration even causes mixing equipment blockage problem, is made troubles to production.Further, since remaining non-volatile moisture is retained in In compound, compound initial performance can be influenceed.The third method is that warm-mixing agent is added in pitch in advance, then take with The same mode of production of common hot-mix asphalt mixture, it is easy to operation, easily received by production unit.This kind of method passes through Warm-mixing agent is added in pitch in advance, reduces the high temperature viscosity of pitch, changes the viscosity-temperature curve of pitch, so as to reduce drip The blue or green mix temperature with building stones, reach warm mix effect.But presently used warm-mixing agent leads to while asphalt high-temperature viscosity is reduced It often can also cause the reduction of 60 DEG C of viscosity of pitch, the high-temperature stability of asphalt is incurred loss；Or on the contrary, do not dropping During low 60 DEG C of viscosity, the loss of pitch ductility can be caused, so as to reduce the cryogenic property of pitch.In a word, it is presently used Warm-mixing agent is while pitch is reached warm mix effect, is high-temperature behavior to lose pitch or cryogenic property as cost 's.

Fischer-Tropsch（F-T）Synthetic technology is nineteen twenty-three invention, mainly includes high temperature synthesis techniques and low temperature synthesis technique, F-T synthesis techniques and catalyst all achieve breakthrough progress since nineteen nineties, and F-T sinteticses are increasingly rich It is rich.In F-T synthetic product chemical compositions based on n-alkane, there is a small amount of isoparaffin, its melt viscosity is low, is crystallized under solid-state Degree is high, can prepare high-melting-point, the wax product of high rigidity, but contains more alkene and oxygenatedchemicals in F-T synthetic products, And carbon number distribution is very wide.Generally F-T waxes are directly used as with the F-T wax oil components synthesized at present to use.

CN200880116167.7（The asphalt modifier for " warm mix " including tackifier）Utilize surfactant group Divide, wax component, resin Composition are prepared for asphalt warm-mix agent.It plays warm mix effect using the lubrication of surface active agent composition Fruit；Wax component（Vegetable wax, animal wax, mineral wax, amide waxe, oxidized wax etc.）Efficient Adhesive Promotion is played with resin Composition, to make up The loss of asphalt viscosity caused by above-mentioned surface active agent composition.Component used in the patent is excessive, and is easy to drop 60 DEG C of viscosity of low pitch, the high-temperature stability of pitch is influenceed, can also reduce the adhesiveness of pitch and building stones.Although the tree of addition Fat component such as rosin, phenolic resin etc. can make up the loss of the asphalt viscosity caused by above-mentioned surface active agent composition, but set Fat component and the compatibility of pitch are bad, easily cause pitch to be layered during long-time storage.

CN201010558295.6（A kind of asphalt mixture warm-mixing modifier and preparation method thereof）Utilize F-T waxes, plasticising Agent, polyacid, synthetic resin, petchem prepare warm mix modifying agent, and wherein F-T waxes are used to reduce asphalt viscosity, and its carbon is former Subnumber is between 40~80（It is preferred that between 45~70）, n-alkane ratio be more than 80%（It is preferred that between 85%~95%）, acid number 0 ~1（It is preferred that between 0~0.5）, fusing point is between 55 DEG C~120 DEG C（It is preferred that between 70~110 DEG C）.The patent does not introduce F-T The source of wax stock, and the F-T wax stocks needle penetration from embodiment（25℃）Only 53.2 dmm are seen, are contained in the F-T wax stocks There is more lower-molecular-weight component, this F-T wax stocks can reduce by 60 DEG C of viscosity of asphaltic products.

CN201110443825.7 discloses a kind of composition for warm-mix asphalt pavements, by 91 ~ 94 mass % pitch, 3 ~ 5 mass % The maleic anhydride grafted polyethylene wax that thermoplastic elastomer (TPE), 2 ~ 4 mass % grafting rate are 4 ~ 10 mass %（MA-g-PE）、0.1~1 Quality % operation oil, viscosity of the said composition at 135 DEG C are no more than 700cp, and said composition meets that the anti-plasticity of high temperature becomes simultaneously The requirement of shape and anti-low-temperature cracking.But the 135 of the bituminous composition DEG C of viscosity are still very big, 135 DEG C of viscosity in embodiment are 675 Cp and 690 cp, and do not provide 135 DEG C of viscosity of matrix pitch and do not add pitch during MA-g-PE to glue as what is compared Degree, can not know mix temperature reduces how many actually, only from the point of view of the 135 DEG C of viscosity numbers provided, and not up to warm mix effect.

CN201010167080.1 discloses a kind of rubber modified asphalt warm-mixing agent, preparation method and application.Warm-mixing agent Form by mass fraction and be：100 parts of water, 5 ~ 30 parts of sodium alkyl sulfate, 15 ~ 30 parts of palmitic acid, 5 ~ 30 parts of oleic acid, dodecyl 1 ~ 20 part of benzene sulfonic acid sodium salt, 1 ~ 15 part of hexadecyltrimethylammonium chloride, Imidazoline Cationic Surfactants ODD10 ~ 30 part.System Preparation Method is that sodium alkyl sulfate, palmitic acid, oleic acid, neopelex, hexadecane are once added in 65 DEG C of water Base trimethyl ammonium chloride, Imidazoline Cationic Surfactants ODD, stir 15 minutes, obtain warm-mixing agent.Can be reduced after use makes With 30 DEG C of asphalt temperature.However, the warm-mixing agent with the addition of substantial amounts of acid and surfactant, meeting etching apparatus, and reducing While pitch temperature in use, the softening point and 60 DEG C of viscosity that can also make pitch reduce, and high-temperature stability is incurred loss.

In existing warm-mixed asphalt preparation process, while asphalt mixture mixing temperature is reduced, it will usually reduce pitch 60 DEG C of viscosity or ductility, so as to have impact on the high-temperature stability of asphalt or low temperature anti-cracking performance.How to use A kind of special warm-mixing agent, without influenceing its high and low temperature performance while asphalt mixing and forming temperature is reduced, turn into A hot issue of warm-mixed asphalt is developed at present.

In terms of wax product production technology, conventional separation manufacturing process mainly has distillation, solvent separation, sweating separation Deng.

Distillation is to reach the purpose of separating-purifying using the boiling point difference of different hydrocarbons, and the boiling range for reducing distillation can be effective The width of product carbon distribution is reduced, but still-process needs raw material being heated to more than boiling point, consumes substantial amounts of energy.Simultaneously The boiling point of hydro carbons of the fusing point more than 70 DEG C is at 500 DEG C（Normal pressure）More than, efficiency is greatly reduced when being separated using distillation.

Solvent fractionation method is to reach separating-purifying using n-alkane and the different solubility of isoparaffin in a solvent Purpose, the normal paraffin content in product can be effectively improved, but the width of carbon distribution is influenceed little, while solvent separates Technique productions equipment investment is big；Need largely to use solvent in production process, recycling design needs to consume substantial amounts of energy；Solvent In contain benzene homologues, environment can be impacted；Solvent is inflammable, easily causes production accident.

Sweating separation method is to carry out separating-purifying using the different property of various component fusing points in wax.Various groups in wax The molecular weight divided Bu Tong can all make its fusing point different with structure.When being all n-alkane, the larger n-alkane of molecular weight Fusing point is higher, and the fusing point of the less n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane To be less than n-alkane, and isomery degree more high-melting-point is lower.

Compared with distillating method, because the melting temperature of various hydro carbons is far below boiling temperature, so sweating separation process Energy consumption be far below separated；Compared with solvent fractionation method, sweating separation process is without using solvent, so sweating separated Cheng Anquan, energy-conservation and on environment without influence.

Common sweating process mainly includes the following steps that：（1）Preparation：Pad water（Sweatbox ware plate is full of with water Lower space）After feed（Load sweatbox when raw material is heated to more than fusing point being in a liquid state）；（2）Crystallization：By raw material with little 10 DEG C~20 DEG C are progressively cooled to below its fusing point in 4 DEG C/h rate of temperature fall.In cooling procedure, various components by fusing point by High to Low order crystallizes to form solid successively；（3）Sweating：After temperature of charge reaches default cooling final temperature, put Fall to pad water；Raw material is slowly heated to default sweating final temperature again.In sweating effort, various components are by fusing point by low Successively liquid is fused into high order and is flowed out（Under wax）, the solid residue that finally obtains（On wax）It is exactly high-melting-point, low The wax of oil-containing, narrow carbon number distribution；Continue to raise temperature, taken out with fusing on wax, as crude product；（4）It is refined：Generally use is white Soil is refined（Predetermined temperature is warming up to after crude product is melted, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the scheduled time）；Pass through again Shaping, packaging are purpose product.

To common sweating separation method, the solids fraction in the sweating effort that heats up（The wax of higher melt）And liquid composition （Oil and the wax compared with low melting point）Although being respectively at two kinds of phases of solid and liquid, it also is difficult to be kept completely separate.It is final to make The oil content of product meets the requirements, and generally use extends sweating sessions and the method for improving sweating final temperature, but can so lead Cause the production cycle long and product yield declines.

Common sweating separating technology can produce fusing point has thick flaky crystal structure under 40 DEG C~60 DEG C of solid-state Soap manufacturing paraffin and low melt point paraffin, be not suitable for producing wax product of the fusing point more than 70 DEG C.Experiment shows that common sweating process is given birth to Fusing point is produced in 70 DEG C or so of wax product, the carbon dispersion of distribution and oil content on sweating later stage wax are unrelated with yield, i.e., on wax The carbon dispersion of distribution and oil content do not decline with the decline of yield, so so far there are no with sweating separating technology production fusing point exist The report of 70 DEG C or so of wax product.

Compared with solvent separating technology, sweating separating technology is intermittently operated, and product yield is relatively low, the production cycle compared with It is long, but sweating process has that small investment, production process are simple, operating cost is low, production process is safe, save and to environment without The advantages that pollution, still there is part producer at present using this method production soap manufacturing paraffin product.

For many years, sweating separation method has obtained some development, such as CN89214332 in production equipment and process aspect（It is vertical Formula square multipul sections spacer diaphoresis tank）、CN94223980.6（Ware type sudorific device）、CN98233254.8（Paraffin sweating pot）、 CN200920033500.X（Novel paraffin sweating tank）、CN201210508905.0（A kind of Efficient paraffin sweatbox）、 CN201320127680.4（Tubular type paraffin deoiler）Deng being improved in sweating production equipment；CN91206202（It is a kind of High-efficient sweat pot for paraffin wax）Improved on sweating separating technology, but these improvement can not still produce fusing point more than 70 DEG C Wax product.

Sweating separating technology is to be currently known unique solvent-free separation method for commercial scale petroleum paraffin product, In promotion green low-carbon, today of environmental protection and energy saving, produced using sweating separating technology while asphalt high-temperature viscosity is reduced not The demand for influenceing the asphalt warm-mix agent product of its applied at elevated temperature performance is more urgent.

CN101735623A discloses a kind of warm mixed epoxy bitumen material and preparation method thereof, including component A and B component.A Component is epoxy resin, and B component includes pitch 40wt%~83wt%, maleic anhydride 5wt%~20wt%, 9- octadecenyl amines 10wt%~30wt%, poly sebacic polyanhydride or poly- azelaic acid acid anhydride 2wt%~10wt%；The mass ratio of component A and B component is 1:3~ 5.8.Medium temperature mix can be used, reduces gas discharge during construction, while it is short to solve general bituminous epoxy operable time Problem.But when preparing B component, maleic anhydride, which is added in pitch, needs stirring 4~6 hours, then also needs to add Add other components, preparation time is oversize, influences production efficiency.In addition, although bituminous epoxy can improve Coating combination, pitch Pitch can be made to become fragile after middle addition epoxy resin, pliability is deteriorated.

CN201510022090.9 discloses a kind of Warm-Mix Bitumen Mixture and preparation method thereof, wherein warm-mixing agent used It is using macromolecule alkane and aromatic naphtha as raw material, and adds halogen and catalyst preparation obtains.Although the patent is in certain journey Solve above mentioned problem on degree, but during warm-mixing agent is prepared, because the reaction temperature of intermediate is low, and lack catalysis Agent, reaction speed is slower, and intermediate activity is relatively low, have impact on the extent of reaction of intermediate and aromatic naphtha, and reaction depth is not allowed yet Easy to control, obtained warm-mixing agent property is unstable, have impact on the application effect in pitch.In addition, the warm-mixing agent preparation process It is complex, the warm-mixing agent is used in pitch, have also appeared the problem of ageing resistace is poor.

During bituminous epoxy is prepared, 60 DEG C of viscosity of bituminous epoxy would generally be caused using current warm mix technology Or ductility reduces, so as to influence the high-temperature stability of epoxy asphalt mixture or low temperature anti-cracking performance.It would therefore be highly desirable to develop Go out a kind of bituminous epoxy, can both reduce temperature in use and solve the problems, such as pliability difference, can also solve high and low temperature performance and The problems such as resistance to heat aging.

The content of the invention

In view of the deficiencies in the prior art, the invention provides a kind of warm mixed epoxy bitumen and preparation method thereof.Pass through addition A kind of special warm-mixing agent, the pliability of bituminous epoxy and the followability with bridge panel can be improved, but also had to pitch There is good warm mix effect, reduce the construction temperature of asphalt, taken into account the high temperature performance of pitch, while can also improve The heat endurance of pitch, improve ageing resistace.

The invention provides a kind of warm mixed epoxy bitumen, including tri- kinds of components of A, B, C, component A therein is warm-mixed asphalt, Warm-mixed asphalt includes warm-mixing agent and matrix pitch；B component is composition epoxy resin；Component C is curing agent；

Described warm-mixing agent is prepared using following methods：

（One）Hydro-conversion：F-T synthetic products carry out hydro-conversion under catalyst action, by alkene therein and oxygen-containing chemical combination Thing is converted into n-alkane；

（Two）Sweating：Including procedure below：

（1）Charging：With（One）Hydroconverted products are raw material, load sweatbox after heating fusing；

（2）Cooling-thermostatical crystallization：With 2.0 DEG C/h~4.0 DEG C/h speed by material be cooled to below raw material melt drop temperature 5 DEG C~ 30 DEG C of cooling final temperature, and constant temperature is for a period of time；

（3）Heating-constant temperature sweating：Heated up with 1.5 DEG C/h~3.5 DEG C/h speed；Material reaches one section of predetermined temperature and constant temperature Stop sweating after time；Forced air flow through in sweating effort material bed；

（4）It is refined：Remaining solids fraction is asphalt warm-mix agent after refined after sweating process.

In the present invention, in described component A warm-mixed asphalt, the addition of warm-mixing agent for warm-mixed asphalt weight 0.4wt%~ 10wt%, preferably 0.5wt%~7.0wt%.

In described component A warm-mixed asphalt, matrix pitch can select the oil drip of various crude oil and different process productions Green grass or young crops, such as the one or more in straight asphalt, oxidized asphalt, solvent deoiling pitch or blend asphalt.

In the present invention, described F-T synthetic products, the requirement of its n-alkane weight content is more than 85%；It is preferred that N-alkanes The F-T synthetic products that hydrocarbon content is more than 95% are as raw material.

In the present invention, process（One）Described hydroconversion process uses the ordinary skill in the art, and its operating condition is： The h of volume space velocity 0.2~2.0 when 3~10MPa of reaction pressure, 150 DEG C~300 DEG C of reaction temperature, liquid^-1, hydrogen liquid volume ratio 100~ 1000:1, hydrogen liquid volume ratio is preferably 300~800:1.Hydrogenation conversion catalyst can be Ni/Al₂O₃、W-Ni/Al₂O₃、Mo- Ni/Al₂O₃Or W-Mo-Ni/Al₂O₃Catalyst etc..Active metal component is using the weight content that oxide is counted as 20% in catalyst ~70%.Hydrogenation conversion catalyst can select existing commercial catalysts, can also be prepared by the conventional method of this area.Urge Reactive metal oxides when in use, can be reduced or vulcanized by this area conventional method as needed, to carry by agent High catalyst activity.

In the present invention, the inorganic of decomposable asymmetric choice net generation gas is preferably mixed under stress after the heating fusing of sweating raw material Salt powder, described pressure（Gauge pressure）Generally 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.Described Inorganic salt powder is in sweating effort, because heated can slowly decompose discharges gas and itself and catabolite and be soluble in Water, can be the one or more in ammonium salt, carbonate, bicarbonate.The granularity of described inorganic salt powder is 50~500 Mesh, addition account for the 0.2%~3.0% of sweating raw material.Inorganic salts are absorbed in the thermostatic process and sweating effort of crystallization and decompose production Raw（It is harmful）Gas.In subtractive process water-washing method can be used to remove unreacted inorganic salts and catabolite.

The preferred sweating ware of heretofore described sweatbox, and increase dismountable sealing system above material and add Pressure device, with step（1）Charging process and step（2）Suppress gas ease caused by inorganic salts decomposition in the temperature-fall period of crystallization Go out material bed.Described pressure（Gauge pressure）For 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.

Described sweating ware increases pressue device above material and/or increases vacuum plant below material.In step （3）In sweating effort, described material bed use that force air flow through increases air pressure above material and/or dropped below material Low pressure, material upper and lower is formed pressure differential and realize.Described pressure differential is generally 0.1~5.0 atmospheric pressure, is preferably 0.2~2.0 atmospheric pressure, it is material bed to force air flow through.

In the present invention, step（2）The rate of temperature fall of the crystallization preferably 2.5 DEG C/h~3.5 DEG C/h.Described cooling terminates Temperature is preferably 10 DEG C~20 DEG C below raw material melt drop temperature.It is described be cooled to final temperature after, the increase constant temperature stage is so that solid Body crystallization is more abundant, and the time in crystallization process constant temperature stage is 0.1~3.0 hour, preferably 1.0~3.0 hours.Crystallization process is permanent Pressure is gradually reduced while warm to normal pressure, rate of pressure reduction is 0.3~8.0 atmospheric pressure/hour.

Step（3）The heating rate of the sweating effort preferably 2.0 DEG C/h~3.0 DEG C/h；The predetermined temperature of the heating For purpose product melt drop temperature -10 DEG C~purpose product melt drop temperature；It is described be warming up to preset temperature after, the increase constant temperature stage so that Solids fraction is sufficiently separated with liquid composition, and the time in constant temperature stage is 0.1~5.0 hour, preferably 1.0~5.0 hours.

In the present invention, during warm-mixing agent is prepared, the programming rate and cooling rate of the material, sky can be passed through Gas bath, water-bath, oil bath or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Using water-bath or oil bath side When formula control material heating rate and rate of temperature fall, chuck, chuck and removable coil pipe and cyclic system can be increased outside sweating ware System be connected, chuck, coil pipe etc. can make material lifting/lowering temperature process faster, temperature of charge evenly；The circulatory system has program drop Temperature/heating function, the circulatory system add the material such as water or conduction oil as circulatory mediator.

During warm-mixing agent is prepared, step（3）Described force air flow through material bed can appoint in sweating effort The meaning stage implements, and preferably implements initial stage in heating sweating.

In the present invention, step（3）Described material bed be utilized in above material that force air flow through increases air pressure realization , it can such as apply 0.2~2.0 atmospheric pressure above material（Gauge pressure）Pressure, and material below remain normal pressure.Or Step（3）Described forcing air flow through is material bed being utilized in material bed lower section reduction air pressure realization, such as can be on material Side keeps normal pressure, and -0.2~-1.0 atmospheric pressure are maintained below material（Gauge pressure）Pressure.

Sweatbox used in the present invention can also connect absorption system, with step（2）The thermostatic process of crystallization And step（3）Absorbed in sweating effort caused by inorganic salts decomposition（It is harmful）Gas.Absorption system uses liquid absorption mode.

Analysis shows, the not impurity such as sulfur-bearing, nitrogen, aromatic hydrocarbons in F-T synthetic products, easily reach very high purity through refined； In the chemical composition of low temperature F-T synthetic products based on n-alkane and distribution is very wide, and containing a small amount of alkene and containing oxidation Compound.The melt viscosity of this product is low, and this is to being beneficial as asphalt warm-mix agent, but due to olefin component be present Asphalt high-temperature stability can be made to be deteriorated；Oxygenatedchemicals has special smell；A large amount of low-melting components make it in asphaltic products 60 DEG C of viscosity of pitch can be reduced during middle use, influence high-temperature stability.Therefore, F-T synthetic products are not suitable for being directly used as dripping Blue or green warm-mixing agent.

Sweating separation method is separated using the fusing point difference of various components.For the research table of sweating effort Bright, liquid composition is gradually discharged along crystalline portion in sweating effort, situation about being flowed similar to liquid in capillary.But It is for high melting-point wax of the fusing point at 70 DEG C or so, because raw material chemical composition is complicated, causes the tiny cause of crystals upon crystallization structure Close, the discharge to liquid composition forms filter flow resistance power, and this is resulted in only by solid in the common sweating effort of gravity natural separation State component is difficult to be kept completely separate with liquid composition, therefore common sweating separating technology can not produce wax production of the fusing point more than 70 DEG C Product.

When preparing the warm-mixing agent used in component A warm-mixed asphalt, by the further investigation of the composition to F-T synthetic products, Contain a certain amount of alkene and oxygenatedchemicals for F-T synthetic products, and be to cause F-T to synthesize containing a large amount of low-melting components The reason for product is not suitable for being directly used as asphalt warm-mix agent, by selecting appropriate catalyst and reaction condition, F-T is synthesized and produced The non-Suitable ingredients such as alkene and oxygenatedchemicals in thing are converted into n-alkane.Pass through deeply grinding to common sweating effort Study carefully, be difficult to liquid composition separate reason for solids fraction, it is material bed using forcing air flow through in sweating effort, and Increase the constant temperature stage in crystallization process and sweating effort；Incorporation can divide under stress further preferably after raw material heating fusing simultaneously The inorganic salt powder of solution generation gas, these measures effectively separate liquid composition with solids fraction, remove F-T synthetic products In low-melting component, product is suitable for use as asphalt warm-mix agent.

The reason for being difficult to separate with liquid composition for solids fraction in sweating effort, by using gas in sweating effort Stream carries out liquid composition by material bed, forces the separation of liquid composition and solids fraction, enhances separating effect and accelerate Separating rate；The inorganic salt powder of decomposable asymmetric choice net generation gas is mixed after the fusing of preferred feedstock heating simultaneously under stress, These materials slowly settle because granularity is smaller in the material of liquid, relatively evenly can be distributed in material.Keep pressure Under the conditions of raw material is cooled to below fusing point 10 DEG C~15 DEG C, and constant temperature 0.1h~3.0h is so that material crystallization is more abundant；Simultaneously Pressure is gradually reduced during cryogenic thermostat to normal pressure.The time that raw material terminates after being cooled to below melt drop temperature to sweating effort In material be in softer solid state, inorganic salts slowly decompose the gas discharged during this, can be formed in material micro- Minute bubbles, the space that these micro-bubbles are formed are easy to form some tiny passages in material in sweating effort, so as to Be advantageous to the discharge of liquid composition in sweating effort.Being aided with the constant temperature stage of crystallization process again makes solid crystal more abundant, and The constant temperature stage of sweating effort makes liquid composition separate the methods of more abundant with solids fraction so that sweating process can produce not Asphalt warm-mix agent containing low-melting component.

In the present invention, described B component is composition epoxy resin, is included in parts by weight：It is 100 parts of epoxy resin, dilute Release 0~40 part of 15~60 parts of agent, 10~30 parts of flexibilizing agent and fiber.

Wherein, described epoxy resin includes：Atmosphere base propane glycidyl ether epoxy resin, Bi-phenolic Methan e shrink sweet Oily ether epoxy resin, more phenolic group propane tetraglycidel ether epoxy resins, aliphatic glycidyl ether epoxy resin, ethylene oxidic ester One or more of mixtures in type epoxy resin, glycidyl amine type epoxy resin；Described diluent includes：Two shrink Glycerin ether, polyglycidyl ether, epoxy propane butyl ether, expoxy propane phenyl ether, diepoxy propane ethylether, three expoxy propane One or more of mixtures in propyl ether, ethanol, acetone, benzene,toluene,xylene；Described flexibilizing agent includes：Polysulfide rubber One or more of mixtures in the tertiary butyraldehyde of glue, polyamide, phenolic resin, polyvinyl alcohol, furfural resin；Described fibre Dimension includes：Asbestos fibre and/or glass fibre.

Described component C is curing agent, and it includes：Ethylenediamine, m-phenylene diamine (MPD), benzene dimethylamine, polyamide, diethylenetriamine In one or more of mixtures.

Described component A and the weight ratio of B component are A:B=3~7:1.The dosage of component C is in B component by weight Content of epoxy resin 0.40%~1.20%, preferably 0.48%~1.05%.

Present invention also offers the preparation method of above-mentioned warm mixed epoxy bitumen, including herein below：Component A is heated to 110 DEG C~130 DEG C, B component is heated to 50 DEG C~80 DEG C, then B component is added in component A while stirring, mixing time It is at least 30min, obtains the mixture of component A and B component；Component C is added in the mixture of component A and B component again, is stirred 3~10min, so as to obtain described warm mixed epoxy bitumen.

Wherein, the preparation method of described component A warm-mixed asphalt comprises the following steps：Matrix pitch is heated to 130 DEG C ~160 DEG C, after complete melting, warm-mixing agent is added while stirring, 30min~60min is stirred, obtains component A warm-mixed asphalt.

The preparation method of described B component composition epoxy resin comprises the following steps：First by epoxy resin, diluent, Flexibilizing agent is heated to 50 DEG C~80 DEG C, is then mixed and stirred for uniformly, finally adding fiber in proportion, is stirred for uniformly.

Another goal of the invention of the present invention is to provide a kind of warm mixed epoxy bitumen compound, wherein containing foregoing warm mix Bituminous epoxy.

The technical scheme is：A kind of warm mixed epoxy bitumen compound, in terms of compound percentage by weight, including with the following group Point：Warm mixed epoxy bitumen 4.0%~6.0%, miberal powder 1.0%~3.0% gather materials 91.0%~95.0%.

It is described gather materials at least one of gather materials selected from limestone, basalt, andesite or granite；It is described to gather materials Proportioning meets any one in close-graded AC-10, AC-13, AC-16 or AC-20.Described miberal powder be by ore grinding and Into wherein particle proportion of the particle diameter less than 0.075mm is more than 70% as mass fraction.

Present invention also offers a kind of preparation method of the warm mixed epoxy bitumen compound, comprise the following steps：70 DEG C~110 DEG C at by warm mixed epoxy bitumen, gather materials, miberal powder stirs, that is, obtain warm mixed epoxy bitumen compound.

Compared with prior art, warm mixed epoxy bitumen of the invention and compound have the following advantages that：

1st, warm mixed epoxy bitumen of the invention, the pliability of conventional bituminous epoxy is not only improved, improved and bridge panel Followability, but also preparation and the construction temperature of bituminous epoxy can be reduced, reduce the generating capacity of pernicious gas, be advantageous to Environmental protection and construction.

2 and with compound made from this warm mixed epoxy bitumen, the Marshall for not only improving epoxy asphalt mixture is stable Degree, Rut resistance and water resistant infringement ability, but also construction temperature can be reduced, reduce the generating capacity of pernicious gas, be advantageous to Environmental protection and construction.

2nd, described warm-mixing agent is homemade warm-mixing agent, when preparing warm-mixing agent, passes through thing using air-flow in sweating effort The bed of material, liquid composition is carried out, enhance the separating effect of liquid composition and solids fraction and accelerate separating rate；Profit simultaneously Gas is also beneficial to the quick outflow of liquid composition in material bed middle formation short space caused by inorganic salts decompose.Obtain Warm-mixing agent not only there is warm mix effect to pitch, but also taken into account the high-temperature behavior of pitch, improved the thermostabilization of pitch Property.

3rd, the special warm-mixing agent that the present invention uses, not only has warm mix effect to pitch, has taken into account the high and low temperature of pitch Can, and the heat endurance of pitch is also improved, improve thermal ageing resistant performance.

4th, method of the invention has that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and without molten The advantages that environment, is polluted in agent.

Embodiment

Technical scheme is described in detail with reference to embodiment, but the invention is not restricted to following examples.Wherein, The wt% being related to is mass fraction.

Embodiment 1

1st, warm-mixing agent is prepared

Including（One）Hydro-conversion and（Two）Sweating two parts.

（One）Hydro-conversion

With the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（Normal paraffin content is 95.5wt%；86.2 DEG C of melt drop temperature；Needle penetration（25℃）55 dmm）For raw material, in FHJ-2 catalyst（A kind of Ni/Al₂O₃Commercially Catalyst, Fushun Petrochemical Research Institute's development and production, active metallic content is counted as 40% using oxide, catalyst is before use Carry out conventional reduction processing）Under effect, in reaction pressure 6.5MPa, 220 DEG C of reaction temperature, volume space velocity 1.0h^-1With hydrogen liquid Product ratio 500:It is hydrogenated with conditions of 1 to convert alkene and oxygenatedchemicals therein.

Hydrogenation products property：N-alkane weight content 97.36%；85.0 DEG C of melt drop temperature；Needle penetration（25℃）57dmm；Color Spectrum-mass spectral analysis, the materials such as alcohol, alkene, acid are not detected.

The materials such as alcohol, alkene, acid are not detected from chromatogram-mass spectral analysis can be seen that the oxygenatedchemicals in raw material has removed； From needle penetration（25℃）57dmm, which can be seen that, contains a large amount of low melting points in hydrogenation products.

（Two）Sweating

This part includes：（1）Preparation,（2）Cooling-thermostatical crystallization,（3）Heating-constant temperature sweating,（4）Product purification etc. Process.

（1）Preparation

Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using conduction oil as Jie Matter；Start the heating function of the circulatory system, conduction oil is warming up to 90 DEG C.Pad water below sweating ware ware plate.

The sealing system on installation sweating ware top simultaneously connects with pressurized buffer tank and compressor；Installed in sweating ware bottom Pressure-reducing cushioning tank simultaneously connects vavuum pump；Start compressor and keep pressurized buffer pressure inside the tank stable in 3.8~4.0 atmospheric pressure （Gauge pressure）.

With（One）Middle hydrogenation products are raw material, are heated to after 90 DEG C of fusings in 3.8~4.0 atmospheric pressure（Gauge pressure）Lower addition Sweating ware.

（2）Cooling-thermostatical crystallization

Start the refrigerating function of the circulatory system, temperature of charge is dropped to 75.0 DEG C and constant temperature 2.0 with 2.5 DEG C/h rate of temperature fall Hour is so that crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank with 5.0 atmospheric pressure/h's by emptying system Rate reduction is to normal pressure.Close the refrigerating function of the circulatory system.

（3）Heating-constant temperature sweating

Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank, to receive the liquid composition of outflow；Start compressor and protect It is stable in 1.1~1.3 atmospheric pressure to hold pressurized buffer pressure inside the tank（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Startup follows Loop system heating function, temperature of charge is set to be increased to 80.0 DEG C with 2.5 DEG C/h heating rate；Stop compressor.

Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.4~-0.6 atmospheric pressure（Gauge pressure）, on material Square air pressure keeps normal pressure；Continue to make temperature of charge be increased to 90.0 DEG C and constant temperature 4.0 hours with 2.5 DEG C/h heating rate so that Liquid composition in material is sufficiently separated with solids fraction.

Stop vavuum pump, terminate sweating effort.Continue the temperature of rise conduction oil to 110 DEG C, make the solid-state group in sweating ware Divide melting outflow, warm-mixing agent crude product is obtained after reception（Ⅰ）.

（4）Product purification

Crude product（Ⅰ）Through washing, it is clay-filtered after be asphalt warm-mix agent（Ⅰ）.

Asphalt warm-mix agent（Ⅰ）Property：93.8 DEG C of melt drop temperature；Needle penetration（25℃）3 dmm.Asphalt warm-mix agent（Ⅰ）Yield is 14.2%（Relative to raw material hydrogenation products）.From needle penetration（25℃）3 dmm can be seen that low melting point is in hydrogenation products It is basic to remove.

2nd, component A warm-mixed asphalt is prepared

7kg warm-mixing agent is weighed, is added to No. 50 solvent deoiling pitches of husky Crude Oil that weight is 93 kg, temperature is 160 DEG C In, 60 min are stirred, obtain described component A warm-mixed asphalt（Numbering A-1）, the property of warm-mixed asphalt is shown in Table 1.

3rd, B component composition epoxy resin is prepared

Weigh atmosphere base propane glycidyl ether epoxy resin 100kg, the kg of diluent diglycidyl ether 15, flexibilizing agent polysulfide The kg of rubber 10, is heated to 50 DEG C, is stirred after mixing；Then the kg of asbestos fibre 40 is weighed, is added in said mixture, Stir, obtain described B component composition epoxy resin（Numbering B-1）.

4th, warm mixed epoxy bitumen is prepared

It is standby to weigh curing agent ethylene diamine 0.48kg（Numbering C-1）.

30 kg A-1 is weighed, is heated to 130 DEG C；10 kg B-1 is weighed, is heated to 50 DEG C；While stirring by B-1 It is added in A-1, after treating all additions, stirs 30min；Then it is further continued for adding above-mentioned load weighted C-1, stirs 3min, obtain warm mixed epoxy bitumen of the present invention.The service condition of warm mixed epoxy bitumen is shown in Table 2.

5th, epoxy asphalt mixture is prepared

According to warm mixed epoxy bitumen, gather materials, the mass ratio of miberal powder be 4: 95 :1 ratio, weigh warm mixed epoxy bitumen, collection Material, miberal powder are simultaneously heated to 110 DEG C.Above-mentioned material is added in stirred tank together, stirs 2 minutes, obtains warm mix ring of the present invention Oxygen asphalt.Then various bitumen mixture specimens are prepared into, performance of asphalt mixture evaluation experimental is carried out, the results are shown in Table 3。

Embodiment 2

1st, warm-mixing agent is prepared

The present embodiment includes：（One）Hydro-conversion and（Two）Sweating two parts.

（One）Hydro-conversion

With the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（Normal paraffin content is 90.0wt%；82.6 DEG C of melt drop temperature；Needle penetration（25℃）62 dmm）For raw material, in catalyst（Mo-Ni/Al₂O₃, in terms of oxide Active metallic content is 20%）Under effect, in reaction pressure 3.0MPa, 300 DEG C of reaction temperature, volume space velocity 2.0h^-1With hydrogen liquid Product ratio 100:It is hydrogenated with conditions of 1 to convert alkene and oxygenatedchemicals therein.

Hydrogenation products property：N-alkane weight content 93.3%；80.6 DEG C of melt drop temperature；Needle penetration（25℃）65 dmm；Color Spectrum-mass spectral analysis, the materials such as alcohol, alkene, acid are not detected.

The materials such as alcohol, alkene, acid are not detected from chromatogram-mass spectral analysis can be seen that the oxygenatedchemicals in raw material has removed； From needle penetration（25℃）65 dmm, which can be seen that, contains a large amount of low melting points in hydrogenation products.

（Two）Sweating

（1）Preparation

Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using conduction oil as Jie Matter；Start the heating function of the circulatory system, conduction oil is warming up to 85 DEG C.Pad water below sweating ware ware plate.

The sealing system on installation sweating ware top simultaneously connects with pressurized buffer tank and compressor；Installed in sweating ware bottom Pressure-reducing cushioning tank simultaneously connects vavuum pump；Pressurized buffer tank emptying system and sweating ware lower exhaust port are connected with absorption system respectively Connect, absorbing medium is used as using 5% NaOH solution.

Start compressor and keep pressurized buffer pressure inside the tank stable in 3.8~4.0 atmospheric pressure（Gauge pressure）.Grind and sieve Separate the sodium acid carbonate of the mesh of 50 mesh~100.

With（One）Middle hydrogenation products are raw material, are heated to after 90 DEG C of fusings in 3.8~4.0 atmospheric pressure（Gauge pressure）Lower incorporation 0.2% foregoing sodium bicarbonate powder, sweating ware is added after being well mixed；Keep pressurized buffer pressure inside the tank stable 3.8~ 4.0 atmospheric pressure.

（2）Cooling-thermostatical crystallization

Start the refrigerating function of the circulatory system, temperature of charge is dropped to 50.0 DEG C and constant temperature 1.0 with 4.0 DEG C/h rate of temperature fall Hour is so that crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank with 8.0 atmospheric pressure/h's by emptying system Rate reduction is to normal pressure.The gas of constant temperature stage discharge decomposes the dioxy generated by 5% NaOH solution to absorb sodium acid carbonate Change carbon.Close the refrigerating function of the circulatory system.

（3）Heating-constant temperature sweating

Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank, to receive the liquid composition of outflow；Start compressor and protect It is stable in 1.1~1.3 atmospheric pressure to hold pressurized buffer pressure inside the tank（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Startup follows Loop system heating function, temperature of charge is set to be increased to 70.0 DEG C with 1.5 DEG C/h heating rate；Stop compressor.

Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.2~-0.4 atmospheric pressure（Gauge pressure）, on material Square air pressure keeps normal pressure；Continue to make temperature of charge be increased to 85.0 DEG C and constant temperature 1.5 hours with 1.5 DEG C/h heating rate so that Liquid composition in material is sufficiently separated with solids fraction.The gas discharged in sweating effort is by 5% NaOH solution, to inhale Receive the carbon dioxide that sodium acid carbonate decomposes generation.

Stop vavuum pump, terminate sweating effort.Continue the temperature of rise conduction oil to 100 DEG C, make the solid-state group in sweating ware Divide melting outflow, warm-mixing agent crude product is obtained after reception（Ⅱ）.

（4）Product purification

Crude product（Ⅱ）Through washing, it is clay-filtered after be asphalt warm-mix agent（Ⅱ）.

Asphalt warm-mix agent（Ⅱ）Property：88.3 DEG C of melt drop temperature；Needle penetration（25℃）2 dmm；Asphalt warm-mix agent（Ⅱ）Yield For 19.0%（Relative to raw material hydrogenation products）.From needle penetration（25℃）2 dmm can be seen that low melting point in hydrogenation products Remove substantially.

2nd, component A warm-mixed asphalt is prepared

0.5kg warm-mixing agents are weighed, are added in No. 90 oxidized asphalts of LIAOHE CRUDE that weight is 99.5 kg, temperature is 140 DEG C, 40min is stirred, obtains described component A warm-mixed asphalt（Numbering A-2）, the property of warm-mixed asphalt is shown in Table 1.

3rd, B component composition epoxy resin is prepared

Weigh glycidyl ester type epoxy resin 100kg, the kg of diluent epoxy propane butyl ether 60, flexibilizing agent phenolic resin 30 Kg, 80 DEG C are heated to, is stirred after mixing, obtain described B component composition epoxy resin（Numbering B-2）.

4th, warm mixed epoxy bitumen is prepared

It is standby to weigh curing agent benzene dimethylamine 1.05kg（Numbering C-2）.

70 kg A-2 is weighed, is heated to 115 DEG C；10 kg B-2 is weighed, is heated to 80 DEG C；B-2 is added while stirring It is added in A-2, after treating all additions, stirs 60min；Then above-mentioned load weighted C-2 is added, stirs 9min, obtains this Invention warm mixed epoxy bitumen.The service condition of warm mixed epoxy bitumen is shown in Table 2.

5th, warm mixed epoxy bitumen compound is prepared

This step obtains warm mixed epoxy bitumen compound, is then prepared into various asphalt examinations with the step 5 of embodiment 1 Part, performance of asphalt mixture evaluation experimental is carried out, the results are shown in Table 3.

Embodiment 3

1st, warm-mixing agent is prepared

Including（One）Hydro-conversion and（Two）Sweating two parts.

（One）Hydro-conversion

With the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（Normal paraffin content is 85.5wt%；80.6 DEG C of melt drop temperature；Needle penetration（25℃）65 dmm）For raw material, in catalyst（W-Ni/Al₂O₃, in terms of oxide Active metallic content is 70%）Under effect, in reaction pressure 10.0MPa, 150 DEG C of reaction temperature, volume space velocity 0.2h^-1With hydrogen liquid Volume ratio 990:It is hydrogenated with conditions of 1 to convert alkene and oxygenatedchemicals therein.

Hydrogenation products property：N-alkane weight content 90.3%；77.0 DEG C of melt drop temperature；Needle penetration（25℃）66 dmm；Color Spectrum-mass spectral analysis, the materials such as alcohol, alkene, acid are not detected.

The materials such as alcohol, alkene, acid are not detected from chromatogram-mass spectral analysis can be seen that the oxygenatedchemicals in raw material has removed； From needle penetration（25℃）66 dmm, which can be seen that, contains a large amount of low melting points in hydrogenation products.

（Two）Sweating

（1）Preparation

Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using conduction oil as Jie Matter；Start the heating function of the circulatory system, conduction oil is warming up to 80 DEG C.Pad water below sweating ware ware plate.

Start compressor and keep pressurized buffer pressure inside the tank stable in 3.8~4.0 atmospheric pressure（Gauge pressure）.Grind and sieve Separate the sodium carbonate of the mesh of 300 mesh~500.

With（One）Middle hydrogenation products are raw material, are heated to after 90 DEG C of fusings in 3.8~4.0 atmospheric pressure（Gauge pressure）Lower incorporation 3% foregoing powdered sodium carbonate, sweating ware is added after being well mixed；Keep pressurized buffer pressure inside the tank stable at 3.8~4.0 Atmospheric pressure.

（2）Cooling-thermostatical crystallization

Start the refrigerating function of the circulatory system, temperature of charge is dropped to 60.0 DEG C and constant temperature 3.0 with 3.0 DEG C/h rate of temperature fall Hour is so that crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank with 6 atmospheric pressure/h speed by emptying system Rate is reduced to normal pressure.The gas of constant temperature stage discharge decomposes the titanium dioxide generated by 5% NaOH solution to absorb sodium acid carbonate Carbon.Close the refrigerating function of the circulatory system.

（3）Heating-constant temperature sweating

Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank, to receive the liquid composition of outflow；Start compressor and protect It is stable in 1.1~1.3 atmospheric pressure to hold pressurized buffer pressure inside the tank（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Startup follows Loop system heating function, temperature of charge is set to be increased to 70.0 DEG C with 3.5 DEG C/h heating rate；Stop compressor.

Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.8~-1.0 atmospheric pressure（Gauge pressure）, on material Square air pressure keeps normal pressure；Continue to make temperature of charge be increased to 77.0 DEG C and constant temperature 3.0 hours with 3.5 DEG C/h heating rate so that Solids fraction in material is sufficiently separated with liquid composition.The gas discharged in sweating effort is by 5% NaOH solution, to inhale Receive the carbon dioxide that sodium acid carbonate decomposes generation.

Stop vavuum pump, terminate sweating effort.Continue the temperature of rise conduction oil to 100 DEG C, make the solid-state group in sweating ware Divide melting outflow, warm-mixing agent crude product is obtained after reception（Ⅲ）.

（4）Product purification

Crude product（Ⅲ）Through washing, it is clay-filtered after be asphalt warm-mix agent（Ⅲ）.

Asphalt warm-mix agent（Ⅲ）Property：86.3 DEG C of melt drop temperature；Needle penetration（25℃）4 dmm；Asphalt warm-mix agent（Ⅲ）Yield For 21.3%（Relative to raw material hydrogenation products）.From needle penetration（25℃）4 dmm can be seen that low melting point in hydrogenation products Remove substantially.

2nd, component A warm-mixed asphalt is prepared

4kg warm-mixing agents are weighed, are added in No. 110 straight asphaltes of Oman's crude oil that weight is 96 kg, temperature is 120 DEG C, are stirred 50min, obtain described component A warm-mixed asphalt（Numbering A-3）, the property of warm-mixed asphalt is shown in Table 1.

3rd, B component composition epoxy resin is prepared

Glycidyl amine type epoxy resin 100kg, the kg of diluent dimethylbenzene 38, the kg of flexibilizing agent furfural resin 20 are weighed, is heated To 65 DEG C, stirred after mixing；Then the kg of glass fibre 20 is weighed, Xu is added in said mixture, stirred slowly, Obtain described B component composition epoxy resin（Numbering B-3）.

4th, warm mixed epoxy bitumen is prepared

It is standby to weigh curing agent polyamide 0.78kg（Numbering C-3）.

50 kg A-3 is weighed, is heated to 120 DEG C；10 kg B-3 is weighed, is heated to 65 DEG C；B-3 is added while stirring It is added in A-3, after treating all additions, stirs 45min；Then above-mentioned load weighted C-3 is added, stirs 6min, obtains this Invention warm mixed epoxy bitumen.The service condition of warm mixed epoxy bitumen is shown in Table 2.

5th, warm mixed epoxy bitumen compound is prepared

Comparative example 1

Weigh the wax oil product of 4kg Sinopec Groups low temperature F-T compound experiment devices（Normal paraffin content For 85.5wt%；80.6 DEG C of melt drop temperature；Needle penetration（25℃）65 dmm）, be directly appended to weight be 96 kg, temperature be 120 DEG C No. 110 straight asphaltes of Oman's crude oil in, stir 50min, obtain a kind of pitch（Numbering W-1）, property is shown in Table 1.Then according to The identical method of the embodiment of the present invention 3 prepares B component composition epoxy resin and component C curing agent；According to the embodiment of the present invention 3 Identical method, with when condition bituminous epoxy is prepared, service condition is shown in Table 2；According to the identical method system of the embodiment of the present invention 3 Standby epoxy asphalt mixture, is then prepared into various bitumen mixture specimens, carries out performance of asphalt mixture evaluation experimental, as a result It is shown in Table 3.

Comparative example 2

B component composition epoxy resin and component C curing agent are prepared according to the identical method of the embodiment of the present invention 3；According to this hair The bright identical method of embodiment 3, with when condition, B component composition epoxy resin and component C curing agent are directly appended to temperature Spend in No. 110 matrix pitches of Oman's crude oil for 130 DEG C, obtain a kind of bituminous epoxy, its service condition is shown in Table 2；According to this hair The bright identical method of embodiment 3 prepares epoxy asphalt mixture, is then prepared into various bitumen mixture specimens, carries out pitch and mixes Material henchnmrk test is closed, the results are shown in Table 3.

The component A warm-mixed asphalt of table 1 contrasts with the property of matrix pitch and comparative example pitch

From table 1, the high temperature viscosity of warm-mixed asphalt of the present invention is all significantly lower than corresponding matrix pitch, so as to be advantageous to drop The construction temperature of low pitch.For warm-mixed asphalt of the present invention compared with corresponding matrix pitch, needle penetration is essentially identical, softening point It is improved significantly with 60 DEG C of viscosity, 10 DEG C of ductilities significantly increase, and illustrate that warm-mixed asphalt of the present invention not only can reach warm mix effect, And corresponding matrix pitch is better than in terms of high-temperature stability and low temperature ductility.

It is visible by comparative example, directly simply the wax oil product of F-T compound experiment devices is added in matrix pitch, Improvement to pitch warm mix effect, be not as good as warm mix effect of the present invention, but also the loss of ductility can be caused, and cause pitch thin Property after film experiment can not reach《Standard specification for construction and acceptance of highway asphalt pavement》JTG F40-2004 technical requirements.And this hair The warm-mixing agent of bright preparation improves the heat endurance of pitch, obtains the ageing resistance of pitch while warm mix effect is realized Improve；And the thermal ageing resistant performance of -1 pair of pitch of comparative example has negative effect.

The service condition of the bituminous epoxy of table 2

Contrasted from table 2, the construction temperature of warm mixed epoxy bitumen of the present invention has obvious reduction, can reduce pernicious gas Amount, and be advantageous to construct；It is significantly better than comparative example with the caking property of floorings, embrittlement temperature is significantly lower than comparative example, illustrates this When invention warm mixed epoxy bitumen is as bridge floor interlaminar bonding material, either cohesive force or flexible aspect is better than comparative example. Also the explanation present invention is improved the thermal ageing resistant performance of pitch, performance also obtains due to having used special warm-mixing agent Improve.

The mix material proportioning of table 3 and property

From table 3, after warm mixed epoxy bitumen of the present invention is added in asphalt, have to Properties of Asphalt Mixture and substantially change Kind, especially Rut resistance and water resistant infringement ability significantly improves.

Claims

1. a kind of warm mixed epoxy bitumen, it is characterised in that the warm mixed epoxy bitumen includes tri- kinds of components of A, B, C, A groups therein It is divided into warm-mixed asphalt, warm-mixed asphalt includes warm-mixing agent and matrix pitch；B component is composition epoxy resin；Component C is solidification Agent；

The warm-mixing agent is prepared using following methods：

（Two）Sweating：Including procedure below

（1）Charging：With（One）Obtained hydroconverted products are raw material, load sweatbox after heating fusing；

（2）Cooling-thermostatical crystallization：With 2.0 DEG C/h~4.0 DEG C/h speed by material be cooled to below raw material melt drop temperature 5 DEG C~ 30 DEG C of final temperature, and constant temperature is for a period of time；

（3）Heating-constant temperature sweating：Heated up with 1.5 DEG C/h~3.5 DEG C/h speed；Material in sweatbox reaches pre- constant temperature Spend and constant temperature stops sweating afterwards for a period of time；Forced air flow through in sweating effort material bed；

（4）It is refined：Remaining solids fraction is by being refining to obtain the warm-mixing agent in sweatbox.

2. warm mixed epoxy bitumen according to claim 1, it is characterised in that n-alkane in described F-T synthetic products Weight content be more than 85%.

3. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（1）In charging process, raw material heating is molten The inorganic salt powder of decomposable asymmetric choice net generation gas is mixed after change under stress.

4. warm mixed epoxy bitumen compound according to claim 3, it is characterised in that described inorganic salts be selected from ammonium salt, One or more in carbonate, bicarbonate.

5. warm mixed epoxy bitumen according to claim 3, it is characterised in that the granularity of described inorganic salt powder be 50~ 500 mesh.

6. warm mixed epoxy bitumen according to claim 3, it is characterised in that the addition of described inorganic salt powder accounts for original Expect the 0.2%~3.0% of weight.

7. warm mixed epoxy bitumen according to claim 3, it is characterised in that in step（1）Charging process and step（2） Apply air pressure above material in the temperature-fall period of crystallization, to suppress gas effusion caused by inorganic salts decomposition.

8. warm mixed epoxy bitumen according to claim 7, it is characterised in that described air pressure is 0.5~15.0 gauge pressure Atmospheric pressure.

9. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（2）Described in the predetermined temperature that cools For 10 DEG C below raw material melt drop temperature~20 DEG C.

10. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（2）Described in the constant temperature stage when Between be 0.1~3.0 hour.

11. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（2）Gradually reduced while constant temperature Pressure is to normal pressure；Rate of pressure reduction is 0.3~8.0 atmospheric pressure/hour.

12. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（3）Described in the predetermined temperature that heats up For purpose product melt drop temperature -10 DEG C~purpose product melt drop temperature.

13. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（3）Constant temperature described in sweating effort Time is 0.1~5.0 hour.

14. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（3）Described in force air flow through It is material bed to implement initial stage in heating.

15. warm mixed epoxy bitumen according to claim 1, it is characterised in that step（3）Described in force air flow through It is material bed to reduce air pressure using in material bed top increase air pressure and/or in material bed lower section, material bed upper and lower is formed pressure Power difference realizes that described pressure differential is 0.1~5.0 atmospheric pressure.

16. warm mixed epoxy bitumen compound according to claim 15, it is characterised in that described forces air flow through thing The bed of material uses to be realized in material bed top increase air pressure, applies the gauge of 0.2~2.0 atmospheric pressure in material bed top, And material bed lower section remains normal pressure.

17. warm mixed epoxy bitumen according to claim 15, it is characterised in that described forces air flow through material bed adopt Used in material bed lower section reduce air pressure realize, material bed top air pressure keep normal pressure, and material bed lower section maintain -0.2~- The gauge of 1.0 atmospheric pressure.

18. warm mixed epoxy bitumen according to claim 3, it is characterised in that in step（2）The thermostatic process and step of crystallization Suddenly（3）Gas caused by inorganic salts decomposition is absorbed using liquid absorption mode in sweating effort, using washing in subtractive process Mode removes unreacted inorganic salts and catabolite.

19. warm mixed epoxy bitumen according to claim 1, it is characterised in that described composition epoxy resin is by weight Number includes：0~40 part of 100 parts of epoxy resin, 15~60 parts of diluent, 10~30 parts of flexibilizing agent and fiber.

20. warm mixed epoxy bitumen according to claim 19, it is characterised in that described epoxy resin includes diphenylol third Alkane tetraglycidel ether epoxy resin, Bi-phenolic Methan e tetraglycidel ether epoxy resin, more phenolic group propane diglycidyl ether epoxy trees One kind in fat, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin Or several mixture；Described diluent includes diglycidyl ether, polyglycidyl ether, epoxy propane butyl ether, epoxy One kind in propane phenyl ether, diepoxy propane ethylether, three expoxy propane propyl ethers, ethanol, acetone, benzene,toluene,xylene Or several mixtures；Described flexibilizing agent includes polysulfide rubber, polyamide, phenolic resin, the tertiary butyraldehyde of polyvinyl alcohol, furfural One or more of mixtures in resin；Described fiber includes asbestos fibre and/or glass fibre.

21. warm mixed epoxy bitumen according to claim 1, it is characterised in that described curing agent includes ethylenediamine, isophthalic One or more of mixtures in diamines, benzene dimethylamine, polyamide, diethylenetriamine.

22. warm mixed epoxy bitumen according to claim 19, it is characterised in that described component A and the weight ratio of B component For A:B=3~7:1；The dosage of component C is 0.40%~1.20% of the content of epoxy resin in B component by weight.

23. the preparation method of any described warm mixed epoxy bitumens of a kind of claim 1-22, it is characterised in that including following step Suddenly：By component A be heated to 110 DEG C~130 DEG C, B component be heated to 50 DEG C~80 DEG C, B component is then added to A while stirring In component, mixing time is at least 30min, obtains the mixture of component A and B component；Again in the mixture of component A and B component Middle addition component C, 3~10min is stirred, so as to obtain described warm mixed epoxy bitumen.

24. preparation method according to claim 23, it is characterised in that the preparation method of described component A warm-mixed asphalt Comprise the following steps：Matrix pitch is heated to 130 DEG C~160 DEG C, after complete melting, warm-mixing agent is added while stirring, stirs 30min~60min is mixed, obtains component A warm-mixed asphalt.

25. preparation method according to claim 23, it is characterised in that the system of described B component composition epoxy resin Preparation Method comprises the following steps：Epoxy resin, diluent, flexibilizing agent are first heated to 50 DEG C~80 DEG C, then mixed in proportion And stir, fiber is finally added, is stirred for uniformly.

A kind of 26. warm mixed epoxy bitumen compound, it is characterised in that in terms of compound percentage by weight, including following components：Power Profit requires the warm mixed epoxy bitumen 4.0%~6.0% described in 1-22 any one, miberal powder 1.0%~3.0%, gather materials 91.0%~ 95.0%。

27. warm mixed epoxy bitumen compound according to claim 26, it is characterised in that described gathers materials selected from lime Rock, basalt, andesite or granite at least one of gather materials；The proportioning gathered materials meet close-graded AC-10, AC-13, Any one in AC-16 or AC-20.

28. warm mixed epoxy bitumen compound according to claim 26, it is characterised in that described miberal powder is ground by ore Mill forms, and wherein particle proportion of the particle diameter less than 0.075mm is more than 70% as mass fraction.

29. the preparation method of the warm mixed epoxy bitumen compound described in claim 26, it is characterised in that at 70 DEG C~110 DEG C It is lower by warm mixed epoxy bitumen, gather materials, miberal powder stirs, obtain warm mixed epoxy bitumen compound.