CN103472091B - A kind of based on the pitch thermal decomposition behavior research method on component level - Google Patents
A kind of based on the pitch thermal decomposition behavior research method on component level Download PDFInfo
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Abstract
The present invention is a kind ofly deep into new method asphalt component level being studied pitch thermal decomposition behavior, belongs to technical field of fire hazard safety, solves the research of current pitch thermal decomposition behavior and is difficult to deep problem.First prepare each component sample, measure each component concentration, adopt differential scanning calorimetry-infrared spectrum technology test pitch and four kinds of component thermal decomposition performances thereof, obtain pitch each component thermal decomposition test figure, analyze composition and the release rule of each component thermal decomposition gradient distribution character and generation flue gas; Secondly, calculate each component Thermal Analysis Kinetics parameter according to Arrhenius equation, set up kinetics of thermal decomposition model; Finally, adopt transmission electron microscope, photoelectron spectrograph to test residue heterogeneous microstructure, composition and content after each component thermal decomposition, each component thermal decomposition behavior of research pitch, and and bitumen samples test findings compare, disclose pitch Thermal Decomposition Mechanism.Method provided by the invention inherently can disclose pitch thermal decomposition behavior in high temperature environments.
Description
Technical field
The present invention is a kind ofly deep into new method asphalt component level being studied pitch thermal decomposition behavior, belongs to asphalt material technical field.
Background technology
In recent years, the fast development of highway in China communication, tunnel also obtains synchronized development as highway important component part.Tunnel can be used in mountainous region overcoming landform and elevation obstacle, improves linear, shortens mileage, improves road speed, preserves the ecological environment.Therefore, be used widely in tunnel in highway engineering, and China has become one of country that Tunnel Engineering is maximum, with the fastest developing speed in the world.Tunnel is to growing up future development, and the volume of traffic increases, and travel speed improves, and tunnel becomes traffic hazard multi-happening section, and the fire failure rate caused thus is in rising trend, and tunnel is faced with severe fire safety evaluating problem.
Along with people require to improve to tunnel road surface safe application performance and fire-retardant, press down cigarette technical progress, bituminous pavement has become the development trend of tunnel road surface because of advantages such as its driving are comfortable, cling property good, noise is little, the construction period is short, easy to maintenance.But pitch is meeting thermal decomposition, burning under fire hazard environment, and discharges a large amount of poison gas and heat, and this seriously hinders tunnel traffic, bring extreme difficulties to trapped personnel escape and fire rescue, cause a tremendous loss of lives.Therefore, the Thermal Decomposition Mechanism in hot environment inquiring into asphalt material seems urgent day by day.
As everyone knows, pitch is very complicated hydro carbons and the potpourri of non-hydrocarbons.Utilize the selective dissolution of pitch in different solvents or the absorption on different adsorbent, be separated into several chemistry, physical property is similar, and have the group of certain relation with its colloform texture character, pavement performance, these groups are just called the component of pitch.Four compositions in current pitch composition partition method has become U.S. ASTM and domestic standard test method, and pitch is divided into saturated point, fragrant point, resin and asphalt four kinds of components by this method, as Fig. 1.
Saturated point by straight chain hydrocarbon, Branched fatty belong to hydrocarbon, alkyl cyclic hydrocarbon and and some alkyl aromaticss form, be a kind of nonpolar thick shape oils, in straw or white.Mean molecular weight is similar to fragrance point, and its composition comprises the saturate of wax and non-wax, comparatively responsive to temperature, in pitch, account for 5% ~ 20%.Fragrance point is made up of the naphthenic aromatic compounds of lowest molecular weight in pitch, and it is the dispersion medium of peptized asphaltenes.Fragrance point accounts for 20% ~ 50% in pitch, is dark-brown thick liquid.Average relative molecular mass is 300 ~ 2000.Fragrance point is made up of non-polar carbon chains, and wherein unsaturation member ring systems is preponderated, and has very strong dissolving power to other macromolecule hydro carbons.In addition, fragrance point and saturated point in pitch as oil content, mainly make colloid-bituminous matter soften (plasticizing), play a part lubrication and solvent, make pitch colloidal dispersion maintenance stablize.Oil content is more responsive to temperature, and its content is more, and the softening point of pitch is lower, and pen. is larger, and denseness reduces.
Colloid is the dark brown solid or the semisolid that are dissolved in normal heptane, is mainly made up of carbon and hydrogen, also has a small amount of nitrogen, sulphur, oxygen.Relative molecular weight is between 1000 ~ 50000, and particle diameter is 1 ~ 5nm.Colloid is bitum diffusant or peptizator, and one of feature of colloid is exactly poor chemical stability, under the impact of adsorbent, heats slightly, and there being air, sunlight is easy to oxidative condensation when existing, and partly becomes bituminous matter.Bituminous matter, except also having some nitrogen, sulphur, oxygen containing except carbon and hydrogen, does not have fixing fusing point, normally first expands during heating, when heating-up temperature arrives more than 300 DEG C, decomposes and generates gas and coke.Relative molecular mass is between 1000 ~ 100000, and particle diameter is 5 ~ 30nm.It is that complicated fragrance divides material, has very strong polarity.Asphalt content is about 5% ~ 25% in most of pitch.
Because scene of fire is not reproducible, the present invention adopts heat analysis method to study asphalt material thermal decomposition behavior.Thermal analyses is under temperature programmed control, utilizes a class technology of the physical property of thermal analyzer measurement of species and the relation of temperature.Wherein, differential scanning calorimetry (DSC) is exactly a kind of thermal analysis system, under programed temperature, measures and is input to the difference power of sample and reference substance and the relation of temperature.The curve that differential scanning calorimeter is recorded to claims DSC curve, it is with the speed of sample neither endothermic nor exothermic, namely rate of heat flow dH/dt (unit MJ/second) is ordinate, with temperature T or time t for horizontal ordinate, the parameter such as specific heat capacity, reaction heat, the heat of transformation, phasor, reaction rate, crystalline rate, crystallinity, sample purity of various material at thermal decomposition process can be measured.This method serviceability temperature wide ranges, resolution is high, sample dosage is few.Be applicable to inorganics, organic compound and Pharmaceutical Analysis.
But differential scanning calorimetry is still very limited to the understanding of the release characteristics that gaseous volatilization in pitch thermal decomposition process divides.In order to deep announcement pitch Thermal Decomposition Mechanism, the present invention adopts differential scanning calorimetry-Fourier transform infrared spectroscopy (DSC-FTIR) coupling technique, this technology is a kind of important tests method of research material thermal stability and thermal decomposition process, can divide the gaseous volatilization discharged in pitch thermal decomposition process and carry out on-line analysis fast, understand the composition of the volatile matter that pitch thermal decomposition process produces.Visible, the maximum advantage of DSC-FTIR is that it can carry out polycomponent on-line analysis simultaneously, and the thermal decomposition of Real-Time Monitoring pitch produces the Changing Pattern of smoke components, deeply discloses pitch thermal decomposition behavior.
The thermal decomposition process of pitch is very complicated, and it is reacted by series of parallel and continuous print and formed, main generation thermal decomposition and thermal polycondensation reaction.Because the material in component each in pitch has similar physicochemical property, show similar Chemical Kinetics characteristic.Oil content is the Light ends in pitch, is molecule the most active in pyrolysis, and therefore first decomposition reaction and polycondensation reaction occur for it, generates the flammable volatile matter of Small molecular and colloid; Colloid is the intermediate component of pitch, is transitional reaction molecular, and reactivity, inferior to oil content, generates the flammable volatile matter of Small molecular and bituminous matter after burning; Bituminous matter is the heavy constituent in pitch, presents larger inertia in pyrolytic process.Pitch thermal decomposition process transforms to the direction of heaviness according to the route of oil content → colloid → bituminous matter → coke.But make their Thermal Analysis Kinetics parameter different owing to having different molecular structures between each component.
In addition, Arrhenius (Arrhenius) equation reflects the temperature variant relation of chemical reaction rate constant.This equation is lnk=lnA-E/RT, and wherein k is rate constant, and R is molar gas constant, and T is thermodynamic temperature, and E is apparent activation energy, and A is pre-exponential factor.Formula makes lnk ~ 1/T figure of experimental data is accordingly a straight line, can obtain apparent activation energy Ea, can obtain pre-exponential factor A by intercept by slope.
At present, less for the research of pitch thermal decomposition behavior under hot environment, pitch is as a kind of charring type organic mixture of complicated component, and its thermal decomposition behavior is deep not enough.Domestic scholars has carried out dsc analysis to pitch, point out that mass loss when pitch is heated mainly occurs in 250 ~ 530 DEG C, and different pitches DSC curve shape basic simlarity, and the thermal change measured when former state pitch state of aggregation changes, have rated temperature stability and the high-temperature behavior of different pitches, propose using pitch spontaneous ignition temperature as define bituminous pavement must occur burn critical temperature.The combustion characteristics of pitch that had researchist by analysis of experiments, points out when fire scale reaches lower than the bituminous pavement that substantially can not ignite during 10MW scale; When fire scale reaches 50MW, bituminous pavement must burn.
Foreign study personnel, by bituminous pavement combustion experiment, propose pitch thermal decomposition starting temperature and are about 300 DEG C, and the kindling point of bituminous pavement between 480 ~ 530 DEG C, and is studied the flue gas toxity that burning produces.Point out the burning behavior of scene of fire bituminous pavement, comprise rate of heat release, flue gas generation etc., bituminous pavement burning is the burning that tunnel fire hazard process pitch is separated out flammable volatile matter and caused.Have scholar to adopt cone calorimetry simulation tunnel fire working, have studied the thermal decomposition characteristic of dissimilar asphalt, result shows burn at tunnel fire hazard process asphalt, and the exhaust gas volumn of rate of heat release, combustion residue and generation is different.
Visible, current pitch Study of Thermal Decomposition Mechanism hypothesis pitch is single, uniform homogeneous blend, and the DSC curve obtained is all too rough, and whole piece DSC curve is regarded as single statistics reaction, obtain unique kinetic parameter, mask some and contribute to the more deep essence understanding pitch thermal decomposition.Moreover the aspect not being deep into asphalt component is studied, does not more inquire into pitch each component kinetics of thermal decomposition capability gradient distribution characteristics, but pitch thermal decomposition process is regarded as an entirety, suppose that thermal decomposition process medium power mathematic(al) parameter is constant.
But, in fact pitch is that four kinds of components that physicochemical property are close mix, the temperature range of often kind of component thermal decomposition is in high temperature environments different, there is notable difference in each component thermal decomposition characteristic of pitch, each component thermal decomposition performance presents obvious gradient distribution, often kind of component makes their pyrolysis Kinetics Parameter different owing to having different molecular structures, set up the Thermal Analysis Kinetics equation that the overall situation is unified, an overall thermal decomposition process can only be reflected, the thermal decomposition behavior of pitch can not be disclosed exactly.
Summary of the invention
(1) technical matters
The object of the invention is to provide a kind of new method based on each component level of pitch being studied pitch thermal decomposition behavior, the method is in conjunction with differential scanning calorimetry and theoretical formula method, solve in the research of current pitch thermal decomposition behavior and there is not deep enough problem, pitch Thermal Decomposition Mechanism in high temperature environments can being disclosed more deeply, providing scientific basis for taking rational flame-retarded technology.
(2) technical scheme
In view of the research method of current existing pitch thermal decomposition behavior exists limitation, the present invention is deep on the level of asphalt component, adopts the method that shop experiment and theoretical formula method combine, the deep essence disclosing the thermal decomposition behavior of pitch.First, according to pitch chemistry constituent test, prepare each component sample respectively, and measure the content of each component of pitch; Then, adopt differential scanning calorimetry to obtain DSC curve, the continuously test findings such as infrared spectrum, charring rate of each component thermal decomposition process of pitch, analyze composition and the release rule of each component thermal decomposition gradient distribution character and each component thermal decomposition generation flue gas; Secondly, calculate each component Thermal Analysis Kinetics parameter according to Arrhenius (Arrhenius) equation, set up pitch each component kinetics of thermal decomposition model; Finally, residue heterogeneous microstructure, composition and content after employing transmission electron microscope, each component thermal decomposition of photoelectron spectrograph test pitch, the each component Thermal Decomposition Mechanism of research pitch, and compare with bitumen samples thermal decomposition result, thus deeply explain pitch Thermal Decomposition Mechanism.
(3) beneficial effect
Thermal decomposition process normally controls the key factor that fire occurs and develops, and the flammable volatile matter that the asphalt pyrolysis stage produces mixes with oxygen in air, when temperature reaches the burning that its kindling point can bring out pitch.Therefore, it is necessary for understanding pitch thermal decomposition behavior feature.Adopt research method provided by the invention can more deep announcement asphalt material Thermal Decomposition Mechanism under the high temperature conditions, the thermal response dynamics of quantitative evaluation pitch thermal decomposition process, for taking suitable asphalt flame-retardant technology to provide important evidence, raising bituminous pavement traffic safety, comfortable, endurance quality are had important practical significance.And this method is simple to operate, highly sensitive, to have fast, accurately and intuitively feature, carry out qualitative and quantitative analysis by DSC curve, the reactive kinetics parameters of important information in relevant sample decomposable process and respective process can be obtained.
Accompanying drawing explanation
Fig. 1 pitch Four composition structure composition schematic diagram
1-saturated point of 2-fragrance point 3-colloid 4-bituminous matter
Embodiment
The method that the present invention adopts shop experiment and theoretical formula method to combine, provide the method based on asphalt component level disclosing pitch thermal decomposition behavior, concrete implementation step is as follows:
(1) the selected bitumen samples that will test, according to existing " highway engineering pitch and Asphalt Mixture Experiment rule (JTGE20-2011) " medium pitch chemical composition test (T0618-1993) relevant regulations, prepare saturated point of pitch, fragrant point, resin and asphalt four kinds of component samples respectively, and measure the content of each component;
(2) pitch and four kinds of each 20mg samples of component thereof are got respectively, adopt DSC-FTIR synchronous analyzers test pitch and four kinds of component thermal decomposition performances thereof, heating rate is 10 DEG C/min, 750 DEG C are risen to from room temperature, atmosphere flow is 100ml/min, obtain the test figure such as DSC, charring rate, continuously infrared spectrum, analyze pitch and four kinds of component thermal properties thereof;
(3) pitch and four kinds of component heat decomposition temperature gradient distributions thereof are analyzed, and utilize DSC curve to calculate the Thermal Analysis Kinetics parameter of pitch and four kinds of components thereof according to Arrhenius (Arrhenius) equation, i.e. activation energy and pre-exponential factor A, the thermal decomposition characteristic of further quantitative comparison pitch and four kinds of components thereof, sets up pitch each component kinetics of thermal decomposition model respectively;
(4) according to the continuous Fourier infrared spectrum obtained, analyze the variation tendency of the composition that produces flue gas in pitch thermal decomposition process and concentration (or temperature) in time, obtain the internal relation between flue gas release rule and pitch thermal decomposition.
(5) residue heterogeneous microstructure, composition and content after employing transmission electron microscope, each component thermal decomposition of photoelectron spectrograph test pitch, understand each component thermal decomposition behavior of pitch, compare with bitumen samples thermal decomposition result, and in conjunction with continuous fourier infrared spectrum row pattern analysis results, deeply disclose pitch Thermal Decomposition Mechanism.
Claims (1)
1. be deep into method asphalt component level being studied pitch thermal decomposition behavior, it is characterized in that the concrete steps of the method are as follows:
(1) the selected bitumen samples that will test, according to existing " highway engineering pitch and Asphalt Mixture Experiment rule (JTGE20-2011) " medium pitch chemical composition test (T0618-1993) relevant regulations, prepare saturated point of pitch, fragrant point, resin and asphalt four kinds of component samples respectively, and measure the content of each component;
(2) pitch and four kinds of each 20mg samples of component thereof are got respectively, adopt DSC-FTIR synchronous analyzers test pitch and four kinds of component thermal decomposition performances thereof, heating rate is 10 DEG C/min, 750 DEG C are risen to from room temperature, atmosphere flow is 100ml/min, obtain DSC, charring rate, continuously infrared spectrum test figure, analyze pitch and four kinds of component thermal properties thereof;
(3) pitch and four kinds of component heat decomposition temperature gradient distributions thereof are analyzed, and utilize DSC curve to calculate the Thermal Analysis Kinetics parameter of pitch and four kinds of components thereof according to Arrhenius (Arrhenius) equation, i.e. activation energy and pre-exponential factor A, the thermal decomposition characteristic of further quantitative comparison pitch and four kinds of components thereof, sets up pitch each component kinetics of thermal decomposition model respectively;
(4) according to the continuous Fourier infrared spectrum obtained, analyze the composition that produces flue gas in pitch thermal decomposition process and concentration in time or the variation tendency of temperature, obtain the internal relation between flue gas release rule and pitch thermal decomposition;
(5) residue heterogeneous microstructure, composition and content after employing transmission electron microscope, each component thermal decomposition of photoelectron spectrograph test pitch, understand each component thermal decomposition behavior of pitch, compare with bitumen samples thermal decomposition result, and in conjunction with continuous fourier infrared spectrum row pattern analysis results, deeply disclose pitch Thermal Decomposition Mechanism.
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| CN104535608A (en) * | 2014-12-15 | 2015-04-22 | 常州大学 | Method for rapidly evaluating activity of catalyst for cyclic ester ring opening polymerization in industrial production process |
| CN104899351B (en) * | 2015-04-23 | 2017-12-12 | 南京林业大学 | Bitumen mixture specimen temperature field analysis method based on discrete element simulation |
| CN105510374A (en) * | 2015-12-08 | 2016-04-20 | 东南大学 | Determination method of asphalt fume in asphalt heating and spontaneous combustion process |
| CN106442950A (en) * | 2016-09-14 | 2017-02-22 | 南京林业大学 | Flame retardation and smoke suppression scheme designing method in whole thermal decomposition process of tunnel asphalt pavement |
| CN106596610A (en) * | 2016-12-19 | 2017-04-26 | 东南大学 | Test method for determining new and old asphalt dissolution index of hot recycled asphalt mixture |
| CN107576587B (en) * | 2017-08-23 | 2020-09-11 | 南京林业大学 | Asphalt aging performance prediction method based on isothermal thermal analysis dynamics |
| CN107365431B (en) * | 2017-08-23 | 2019-08-06 | 南京林业大学 | Compound age resister preparation method based on pitch each component thermo-oxidative ageing |
| CN107421844B (en) * | 2017-08-23 | 2021-01-05 | 南京林业大学 | Short-term aging simulation method for components of asphalt based on thermal analysis-infrared combination |
| CN109060878A (en) * | 2018-08-22 | 2018-12-21 | 南京林业大学 | Asphalt component Evaluation of Thermal Stability method based on kinetics of combustion parameter |
| CN109060880A (en) * | 2018-08-23 | 2018-12-21 | 南京林业大学 | A kind of flame retardant efficiency of asphalt evaluation method based on Thermal Analysis Kinetics parameter |
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Application publication date: 20131225 Assignee: Nanjing Shangdu Highway Maintenance Technology Co., Ltd. Assignor: Nanjing Forestry University Contract record no.: 2018320000316 Denomination of invention: Component level-based asphalt thermal decomposition behavior researching method Granted publication date: 20151125 License type: Common License Record date: 20181114 Application publication date: 20131225 Assignee: GANSU CHANGHENG HIGHWAY MAINTENANCE TECHNOLOGY CO., LTD. Assignor: Nanjing Forestry University Contract record no.: 2018320000317 Denomination of invention: Component level-based asphalt thermal decomposition behavior researching method Granted publication date: 20151125 License type: Common License Record date: 20181114 |
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Application publication date: 20131225 Assignee: Jiangsu Dingzhou Transportation Technology Co., Ltd Assignor: Nanjing Forestry University Contract record no.: X2019320000275 Denomination of invention: Component level-based asphalt thermal decomposition behavior researching method Granted publication date: 20151125 License type: Common License Record date: 20191118 |
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