CN104697916B - Method for recognizing and analyzing single particle of solid fuel particles - Google Patents
Method for recognizing and analyzing single particle of solid fuel particles Download PDFInfo
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- CN104697916B CN104697916B CN201510020202.7A CN201510020202A CN104697916B CN 104697916 B CN104697916 B CN 104697916B CN 201510020202 A CN201510020202 A CN 201510020202A CN 104697916 B CN104697916 B CN 104697916B
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Abstract
The invention discloses a method for recognizing and analyzing a single particle of solid fuel particles. The method comprises the following steps: analyzing an ash sample collected after the combustion of solid fuels by utilizing a CCSEM (computer control scanning electron microscope) technique, converting the geometric particle size of each ash particle determined via the CCESM technique by a particle size conversion formula into aerodynamic diameter, thus recognizing particulate matters at each particle size section in flying ash, such as PM0.5-10, PM0.5-2.5 and PM2.5-10 at the particle diameter size section of 0.5-10microns of the representative aerodynamic diameter; and analyzing the particle size of ash particles and the mineral composition information, thereby obtaining the mineral composition of PM0.5-2.5 and PM2.5-10 respectively, the enrichment situation of typical minerals in ash in PM0.5-2 and PM2.5-10 as well as the occurrence mode of typical ash formation elements in particulate matter at each particle size section. According to the method, the single particle of the particulate matter is counted and recognized by utilizing the advantages of the CCSEM technique in statistics via the particle size conversion method, and the theoretical and technical guidance can be provided for the establishment and analysis of important parameters of solid fuel particles, such as the source, the element occurrence mode.
Description
Technical field
The invention belongs to clean combustion and pollutant emission control technology field, and in particular to a kind of to solid fuel ignition
The ash particle of generation carries out single particle analysis, to recognize method of the particulate matter with its individual particle physico-chemical property is analyzed, especially suitable
In solid fuel of bituminous coal, anthracite and other volatile matter contents of the ash amount containing Fe less than 5% less than 30%.
Background technology
Pellet (PM in air10, the general name of the particulate matter of equivalent aerodynamic diameter≤10 μm), especially
Fine particle (PM2.5, aerodynamic diameter≤2.5 μm) high-load be considered as that the chief-criminal for causing China's city haze brings disaster upon
It is first.The burning of the solid fuels such as thermal coal is one of important source of China's Particulate Pollution, and the solid with coal as representative is fired
After material burning, the deep development of particulate matter Treatment process has been the major issue for being related to national economy.
It is effectively to recognize its source, air to the analysis that particulate matter carries out the physico-chemical properties such as individual particle particle diameter, elemental composition
Propagation characteristic, element occurrence patterns and pathogenic etc. important prerequisite, but realize particulate matter single particle analysis also exist it is larger
It is difficult.By advanced PM10Analytical technology means, such as low pressure ram (Low Pressure Impactor, LPI), can obtain
The physico-chemical properties such as the total quality of each particle diameter section particulate matter, elemental composition, can by the scanning electron microscope (SEM-EDS) for being furnished with power spectrum
To PM10Carry out individual particle chemical composition analysis.But, the physico-chemical property for obtaining a large amount of granules could realize list on statistical significance
The sign of granule physico-chemical property., due to inferior positions such as manual operation, naked eyes identification granules, efficiency is very low for traditional SEM-EDS technologies.
And computer controls scanning electron-microscopy (Computer-Controlled Scanned Electron Microscope,
CCSEM single particle analysis can be carried out within a short period of time to 2000-3000 granule of same sample), therefore has the ability to realize
PM10Efficiently, the single particle analysis on statistical significance.
The content of the invention
Deficiency of the present invention for current particulate matter single particle analysis technology, there is provided a kind of to single of solid fuel particle thing
Grain identification and the method for analysis, realize to PM10Mineral composition, mineral distribution, the analysis of the feature such as element occurrence patterns, the party
Method can greatly deepen the understanding to particulate matter physico-chemical property after the solid fuel ignition with coal as representative.
To achieve these goals, a kind of side solid fuel particle thing individual particle recognized with analysis that the present invention is provided
Method, comprises the following steps：
(1) ash sample after solid fuel ignition is collected, using the several of computer controls scanning electron microscope analysis each ash particles
What particle diameter, elemental composition, mineral species and content；
(2) using geometry particle diameter and the reduction formula of aerodynamic diameter, each ash particle that step (1) is obtained
Geometry particle diameter is scaled aerodynamic diameter；
(3) identify ash particle of the aerodynamic diameter in each particle diameter section；
(4) ash particle of each particle diameter section that step (3) is identified and the low pressure ram based on aerodynamic principle
The ash particle of the corresponding particle diameter section of collection makees the contrast of mass size distribution, or using ash in scanning electron microscope analysis correspondence particle diameter section
Whether the number ratio of born of the same parents' granule, checking particle diameter conversion method are effective, for effective solid-fuel sample enters (5th) step；
(5) physico-chemical property analysis is carried out to the individual particle of each particle diameter section using the statistical result of step (3), including analysis is respectively
The mineral composition of particle diameter section particulate matter and content；Analyze preservation situation of the specific mineralogical composition in each particle diameter section particulate matter；
Analyze preservation situation of the main Ash forming elements in each particle diameter section of particulate matter, each mineralogical composition.
The solid of high-order coal or other volatile matter contents of the present invention for ash amount containing Fe less than 5% less than 30% fires
Material, collects the ash sample after burning；By particle diameter reduction formula, the geometry particle diameter that CCSEM analyzes gained ash sample is scaled into air
Kinetic diameter, realizes the identification of particulate matter, that is, identify the particulate matter of multiple particle diameter sections, such as representative air force
Learn the PM of 0.5-10 μm of particle diameter section of diameter0.5-10, and PM0.5-2.5And PM2.5-10Deng；To PM0.5-10Single particle analysis are carried out, it is real
The now mineral composition to each particle diameter section particulate matter, certain minerals composition preservation situation in each particle diameter section particulate matter, mainly into ash
Element analysis such as occurrence patterns in each particle diameter section of particulate matter, each mineralogical composition.
In a word, the present invention is by particulate matter after CCSEM technologies identification solid fuel ignition and analyzes its physico-chemical property, to combustion
Burning the flying dust for generating carries out single particle analysis, realizes to PM0.5-10The identification of individual particle and the analysis of physicochemical characteristic, are fully understood by
Solid fuel ignition generates the physical chemical characteristicses on particulate matter statistical significance, is source, the element preservation of solid fuel particle thing
The foundation of the important parameters such as form provides theoretical and technological guidance with analysis.
Description of the drawings
Fig. 1 is the PM that CCSEM identifications are collected with LPI0.5-10Mass size distribution schematic diagram；
Fig. 2 is PM0.5-2.5、PM2.5-10With complete grey respective mineral composition schematic diagram；
Fig. 3 is PM0.5-10And typical mineral composition each particle diameter section Mass Distribution schematic diagram in 10 μm；
Fig. 4 is Mass Distribution schematic diagram of the Fe elements in grey (particulate matter) each mineralogical composition.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples pair
The present invention is described in detail.It should be appreciated that specific embodiment described herein is only to explain the present invention, but the present invention
Do not limited by this embodiment.
It is a kind of to method of the particulate matter individual particle identification with analyzing, its step bag after solid fuel ignition that the present invention is provided
Include：
(1) collect solid fuel ignition after ash sample, using computer controls scanning electron microscope (CCSEM) technical Analysis each
The geometry particle diameter of ash particle, elemental composition, mineral species and content；
Jing meltings, cooling, grinding, polishing after flying dust is uniformly mixed with Brazil wax, are obtained the good sample of dispersion
Product, obtain the backscatter images of sample in environmental scanning electronic microscope；Choose enough picture numbers and obtain 2000-3000 ash
The data of grain, to meet the analysis of statistical significance；The analysis in power spectrum " Particles " function obtains the several of each ash particle
What particle diameter and inorganic elementss composition；Each ash particle is divided to into specific ash mineral species by elementary composition, the species owns
The quality of granule and it is content of the mineralogical composition in ash.
(2) it is using the analysis result of step (1), just every with the reduction formula of aerodynamic diameter using geometry particle diameter
The geometry particle diameter of individual ash particle is scaled aerodynamic diameter；Geometry particle diameter d and aerodynamic diameter daerReduction formula
ForAsh particle density p takes the corresponding density value of the defined mineral species of step (1).
(3) particulate matter of each particle diameter section, such as 0.5-10 μm of particle diameter section of aerodynamic diameter are may recognize that using step (2)
Particulate matter, be designated as PM0.5-10, and the particulate matter of various typical particle diameter sections, such as PM0.5-2.5、PM2.5-10Deng.
It should be noted that being limited by the technology acuracy of scanning electron microscope, superfine particulate matter within 0.5 μm cannot be realized at present
Single particle analysis.
(4) two ways can be adopted to confirm the effectiveness of particle diameter scaling results：One is using based on aerodynamic principle
LPI collect PM10, its PM recognized with step (3)0.5-10Make the contrast of mass size distribution with verify CCSEM tests with
The effectiveness of grain particle diameter conversion；Two to observe the presence situation of the mellow lime born of the same parents' granule of scanning electron microscope shape appearance figure, and the presence of grey born of the same parents can be led
Ash particle density is caused to have difference with reduction formula input value.
When 20% is less than per grade particles thing data deviation in mass size distribution in " verification mode one " be considered there is effect
Card；After " verification mode two " observation shape appearance figure, when grey born of the same parents' numbers of particles accounts for total ash particle ratio less than 10%, it is believed that be have effect
Card.Multiple data test results show that ash amount containing Fe is less than the high-order coals such as 5% bituminous coal, anthracite, and volatile matter content
Less grey born of the same parents' granule, and particle diameter scaling results and LPI test result bases are produced after other solid fuel ignitions less than 30%
This coincide, therefore is applied to this reduction formula.Two kinds of verification modes can be chosen any one kind of them, invalid solid-fuel sample after checking
Then think not being suitable for the method.
(5) Jing after step (4) checking to PM0.5-10Individual particle physico-chemical property be analyzed.Known based on step (1)-(3)
The aerodynamic diameter and mineral species, content of each ash particle, is not obtained the mineral of each particle diameter section particulate matter after collecting
Composition, such as PM0.5-2.5And PM2.5-10Respective mineral species and content, and certain specific mineralogical composition species is in each particle diameter section
Preservation situation in particulate matter.The elementary composition of each ash particle is recognized based on step (1), certain element is calculated in the ash particle
Quality, after collecting the aerodynamic diameter and mineralogical composition species data of each ash particle, main Ash forming elements can be analyzed
Preservation situation in each particle diameter section of particulate matter, each mineralogical composition.
Example：
The method to the identification of particulate matter individual particle and analysis after solid fuel ignition disclosed in the present embodiment, concrete steps
It is as follows：
(1) fuel selected by the present embodiment is a kind of typical steam coal：Yangquan anthracite, collects coal dust and advises in laboratory
Ash sample 1300 DEG C in mould sedimentation furnace, after air atmosphere burning.
(2) using CCSEM technical Analysis ash samples, the concrete grammar of analysis is：Flying dust sample is obtained in environmental scanning electronic microscope
Product clearly backscatter images, obtain the geometry particle diameter of each ash particle；Energy spectrum analysiss are carried out to ash particle and obtains individual particle
Inorganic elementss are constituted；Enough picture numbers are chosen in power spectrum " Particles " function, to ensure that computer is automatic to sample
Analysis meets 2000-3000 ash particle of statistical calculations meaning；Each ash particle elementary composition is divided to as respective
Specific mineral species；The all ash particle quality for being defined as mineral of the same race add and are the content of the grey mineralogical composition.
(3) using the analysis result of step (2), using geometry particle diameter d and aerodynamic diameter daerReduction formulaThe geometry particle diameter of each ash particle is scaled into aerodynamic diameter, ash particle density p takes step (2)
The density value of defined mineral, thus may recognize that PM0.5-10。
(4) PM is collected using LPI10, its PM recognized with step (3)0.5-10Make mass fraction grain in the range of same particle size
The contrast of footpath distribution, as shown in figure 1, the PM that two methods are collected0.5-2.5Particle diameter distribution is closely similar, 2.5-10 μ ms
Grain thing differing distribution is relatively bigger, it may be possible to grey impact of born of the same parents' granule to reduction formula accuracy in part；In general, the example
The particle diameter distribution that lower two methods are obtained is coincide good.Scanning electron microscope shape appearance figure there's almost no grey born of the same parents in displaying that ash sample
Grain, each grey mineralogical composition density value adopted on reduction formula affect very little.
(5) PM is recognized using step (1)-(3)0.5-10, and confirm the effectiveness of the particle diameter conversion method using step (4)；
Subsequently to PM0.5-10Individual particle physical chemical characteristicses made a concrete analysis of.
Fig. 2 analyzes the mineral composition of each particle diameter section particulate matter, with PM0.5-2.5、PM2.5-10As a example by full ash sample, as a result table
It is bright, PM0.5-2.5Main grey mineralogical composition is Fe aluminosilicates, mixes aluminosilicate and difficult identification composition, and PM2.5-10Master
Amount mineralogical composition is mullite and Fe aluminosilicates.
Fig. 3 analyzes preservation situation of the certain minerals composition in each particle diameter section particulate matter, with PM0.5-10The comparison of distribution can
It was found that, it is enriched in Fe aluminosilicates below 2.5 μm of granules more, and mullite phase constituent is then present in thicker of 2.5-10 μm more
Grain particle diameter section.
Fig. 4 analyzes preservation situation of the Ash forming elements in each particle diameter section of particulate matter, each mineralogical composition, by taking Fe elements as an example,
Fe is in PM0.5-2.5In be present in Fe aluminosilicates and difficult identification composition more；PM2.5-10In Fe be distributed in Fe aluminosilicates, Mo Lai
Content in stone and difficult identification composition is larger.
The invention is not restricted to the restriction of embodiment, be equally applicable to coal of the ash amount containing Fe less than 5% and contain with volatile matters
Solid fuel of the amount less than 30%.The above, a kind of specific embodiment only of the invention, but the scope of protection of the invention
It is not limited thereto.Any those familiar with the art the invention discloses technical scope in, can readily occur in
Change or replacement, should all be included within the scope of the present invention.
Claims (4)
1. a kind of method to the identification of solid fuel particle thing individual particle with analyzing, comprises the following steps：
(1) ash sample after solid fuel ignition is collected, using the geometry grain of each ash particle of computer controls scanning electron microscope analysis
Footpath, elemental composition, mineral species and content；
(2) using geometry particle diameter and the reduction formula of aerodynamic diameter, the geometry of each ash particle that step (1) is obtained
Particle diameter is scaled aerodynamic diameter；
(3) identify ash particle of the aerodynamic diameter in each particle diameter section；
(4) what the ash particle and the low pressure ram based on aerodynamic principle that step (3) is identified each particle diameter section was collected
The ash particle of correspondence particle diameter section makees the contrast of mass size distribution, or using grey born of the same parents' granule in scanning electron microscope analysis correspondence particle diameter section
Number ratio, checking particle diameter conversion method whether effectively, for effective solid-fuel sample enters the 5th step；
(5) the individual particle materialization property analysis using the statistical result of step (3) to each particle diameter section, including analyze each particle diameter section
The mineral composition of grain thing and content；Analyze preservation situation of the specific mineralogical composition in each particle diameter section particulate matter；Analysis is main
Preservation situation of the Ash forming elements in each particle diameter section of particulate matter, each mineralogical composition.
2. method according to claim 1, it is characterised in that in the step (1), using computer controls scanning electron microscope
The method of analysis ash particle is as follows：Flying dust and Brazil wax are uniformly mixed to prepare into sample, flying dust is obtained in scanning electron microscope
Backscatter images；Choose enough picture numbers to obtain 2000-3000 ash particle for meeting statistical analysis, then analyze every
The geometry particle diameter of individual ash particle and elementary composition.
3. method according to claim 1, it is characterised in that：For to including PM0.5-2.5、PM2.5-10And PM0.5-10Including
It is arbitrary or appoint several particle diameter sections particulate matter counted respectively and analyzed.
4. method according to claim 1, it is characterised in that：It is suitable for fuel and the bituminous coal, the nothing that are less than 5% is measured containing Fe for ash
The solid fuel of bituminous coal and other volatile matter contents less than 30%.
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| CN101498647A (en) * | 2009-03-20 | 2009-08-05 | 北京师范大学 | Micro-beam X-ray fluorescence equipment used for atmosphere particle single-particle analysis |
| CN103454203A (en) * | 2013-09-09 | 2013-12-18 | 中国科学院合肥物质科学研究院 | Real-time online measurement system and method of particle size and chemical components of atmospheric particulate |
| CN103592207A (en) * | 2013-11-18 | 2014-02-19 | 华中科技大学 | Method for identifying slagging trend of different mineral components in coal ash |
| CA2831108A1 (en) * | 2012-10-26 | 2014-04-26 | Pratt & Whitney Canada Corp. | Method and system for failure prediction using lubricating fluid analysis |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498647A (en) * | 2009-03-20 | 2009-08-05 | 北京师范大学 | Micro-beam X-ray fluorescence equipment used for atmosphere particle single-particle analysis |
| CA2831108A1 (en) * | 2012-10-26 | 2014-04-26 | Pratt & Whitney Canada Corp. | Method and system for failure prediction using lubricating fluid analysis |
| CN103454203A (en) * | 2013-09-09 | 2013-12-18 | 中国科学院合肥物质科学研究院 | Real-time online measurement system and method of particle size and chemical components of atmospheric particulate |
| CN103592207A (en) * | 2013-11-18 | 2014-02-19 | 华中科技大学 | Method for identifying slagging trend of different mineral components in coal ash |
Non-Patent Citations (2)
| Title |
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| 煤粉热解过程对PM_0_1_内元素成分的影响;温昶 等;《动力工程学报》;20110531;第31卷(第5期);第375-380页 * |
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