CN104697916A - 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 PDF

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CN104697916A
CN104697916A CN201510020202.7A CN201510020202A CN104697916A CN 104697916 A CN104697916 A CN 104697916A CN 201510020202 A CN201510020202 A CN 201510020202A CN 104697916 A CN104697916 A CN 104697916A
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particle size
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solid fuel
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CN104697916B (en
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温昶
徐明厚
于敦喜
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Huazhong University of Science and Technology
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Abstract

本发明公开了一种对固体燃料颗粒物单颗粒识别与分析的方法,其利用计算机控制扫描电镜技术(CCSEM)分析固体燃料燃烧后收集的灰样,由粒径换算公式将CCSEM所测每个灰颗粒的几何粒径换算为空气动力学直径,可识别出飞灰中各粒径段的颗粒物,如具有代表性的空气动力学直径0.5-10μm粒径段的PM0.5-10,以及PM0.5-2.5和PM2.5-10等。通过分析灰颗粒的粒径与矿物组成信息,可得到PM0.5-2.5和PM2.5-10各自的矿物组成,灰中典型矿物在PM0.5-2.5和PM2.5-10中的富集情况;还可得到各粒径段颗粒物中典型成灰元素的赋存形态。本发明通过粒径换算的方法,应用CCSEM技术统计学上的优势实现了颗粒物的单颗粒统计与识别,可为固体燃料颗粒物的来源、元素赋存形态等重要参数的建立与分析提供理论与技术指导。

The invention discloses a method for identifying and analyzing single particles of solid fuel particles. It uses computer-controlled scanning electron microscopy (CCSEM) to analyze the ash samples collected after solid fuel combustion, and uses the particle size conversion formula to convert each ash sample measured by CCSEM to The geometric particle size of the particles is converted to the aerodynamic diameter, which can identify the particles of each particle size in the fly ash, such as PM 0.5-10 in the typical aerodynamic diameter of 0.5-10μm particle size, and PM 0.5- 2.5 and PM 2.5-10 etc. By analyzing the particle size and mineral composition information of ash particles, the respective mineral compositions of PM 0.5-2.5 and PM 2.5-10 can be obtained, and the enrichment of typical minerals in the ash in PM 0.5-2.5 and PM 2.5-10 can also be obtained. The occurrence forms of typical ash-forming elements in the particles of each particle size range were obtained. The present invention realizes single particle statistics and identification of particulate matter through the method of particle size conversion, and applies the statistical advantages of CCSEM technology, which can provide theory and technology for the establishment and analysis of important parameters such as the source of solid fuel particulate matter and the occurrence form of elements. guide.

Description

一种对固体燃料颗粒物单颗粒识别与分析的方法A method for single particle identification and analysis of solid fuel particulate matter

技术领域technical field

本发明属于洁净燃烧和污染物排放控制技术领域,具体涉及一种对固体燃料燃烧产生的灰颗粒进行单颗粒分析,以识别颗粒物与分析其单颗粒物化性质的方法,尤其适用于灰分含Fe量低于5%的烟煤、无烟煤及其它挥发分含量低于30%的固体燃料。The invention belongs to the technical field of clean combustion and pollutant emission control, and specifically relates to a method for single-particle analysis of ash particles produced by solid fuel combustion to identify particulate matter and analyze the physical and chemical properties of the single particle, and is especially suitable for the Fe content in ash Less than 5% bituminous coal, anthracite and other solid fuels with a volatile content of less than 30%.

背景技术Background technique

大气中可吸入颗粒物(PM10,空气动力学当量直径≤10μm的颗粒物的总称),尤其是细颗粒物(PM2.5,空气动力学直径≤2.5μm)的高含量被认为是造成我国都市雾霾的罪魁祸首。动力煤等固体燃料的燃烧是我国颗粒物污染的重要源头之一,对以煤为代表的固体燃料燃烧后颗粒物治理技术的深度开发已是关系到国计民生的重要问题。The high content of inhalable particulate matter (PM 10 , the general term for particles with an aerodynamic equivalent diameter ≤ 10 μm), especially fine particulate matter (PM 2.5 , aerodynamic diameter ≤ 2.5 μm) in the atmosphere is considered to be the cause of urban smog in China. the culprit. The combustion of solid fuels such as thermal coal is one of the important sources of particulate matter pollution in my country, and the in-depth development of particulate matter control technology after solid fuel combustion represented by coal is an important issue related to the national economy and people's livelihood.

对颗粒物进行单颗粒粒径、元素成分等物化性质的分析是有效识别其来源、空气传播特征、元素赋存形态及致病性等的重要前提,但实现颗粒物的单颗粒分析还存在较大困难。借助先进的PM10分析技术手段,如低压撞击器(Low Pressure Impactor,LPI),能得到各粒径段颗粒物总的质量、元素成分等物化性质,借助配有能谱的扫描电镜(SEM-EDS)能够对PM10进行单颗粒化学成分分析。但是,得到大量颗粒的物化性质才能实现统计学意义上单颗粒物化性质的表征。传统的SEM-EDS技术由于手动操作、肉眼识别颗粒等劣势,效率很低。而计算机控制扫描电镜技术(Computer-Controlled Scanned Electron Microscope,CCSEM)能够在较短时间内对同一样品2000-3000个颗粒进行单颗粒分析,因此有能力实现PM10高效的、统计学意义上的单颗粒分析。The analysis of physical and chemical properties such as single particle size and element composition of particulate matter is an important prerequisite for effectively identifying its source, airborne characteristics, element occurrence form, and pathogenicity, but there are still great difficulties in realizing single particle analysis of particulate matter . With the help of advanced PM 10 analysis techniques, such as Low Pressure Impactor (LPI), the physical and chemical properties such as the total mass and elemental composition of particles in each particle size segment can be obtained, and the scanning electron microscope (SEM-EDS ) can analyze the chemical composition of PM 10 in a single particle. However, the physical and chemical properties of a large number of particles can be obtained to achieve the characterization of the physical and chemical properties of a single particle in a statistical sense. Traditional SEM-EDS technology is inefficient due to the disadvantages of manual operation and naked eye identification of particles. However, Computer-Controlled Scanned Electron Microscope (CCSEM) can perform single particle analysis on 2000-3000 particles of the same sample in a relatively short period of time, so it has the ability to achieve efficient and statistically single particle analysis of PM10 . particle analysis.

发明内容Contents of the invention

本发明针对目前颗粒物单颗粒分析技术的不足,提供一种对固体燃料颗粒物单颗粒识别与分析的方法,实现对PM10的矿物组成、矿物分布、元素赋存形态等特征的分析,该方法可以极大深化对以煤为代表的固体燃料燃烧后颗粒物物化性质的认识。The present invention aims at the deficiency of the current particle single particle analysis technology, and provides a method for identifying and analyzing the solid fuel particle single particle, and realizes the analysis of the mineral composition, mineral distribution, element occurrence form and other characteristics of PM 10. The method can Greatly deepen the understanding of the physical and chemical properties of particulate matter after solid fuel combustion represented by coal.

为了实现上述目的,本发明提供的一种对固体燃料颗粒物单颗粒识别与分析的方法,包括以下步骤:In order to achieve the above object, the present invention provides a method for identifying and analyzing solid fuel particulate single particles, comprising the following steps:

(1)收集固体燃料燃烧后的灰样,利用计算机控制扫描电镜分析每个灰颗粒的几何粒径、元素成分、矿物种类与含量;(1) Collect the ash samples after solid fuel combustion, and analyze the geometric particle size, elemental composition, mineral type and content of each ash particle with a computer-controlled scanning electron microscope;

(2)采用几何粒径与空气动力学直径的换算公式,将步骤(1)得到的每个灰颗粒的几何粒径换算为空气动力学直径;(2) adopt the conversion formula of geometric particle diameter and aerodynamic diameter, the geometric particle diameter of each ash particle that step (1) obtains is converted into aerodynamic diameter;

(3)识别出空气动力学直径在各粒径段的灰颗粒;(3) Identify the ash particles whose aerodynamic diameter is in each particle size segment;

(4)将步骤(3)识别出的各粒径段的灰颗粒与基于空气动力学原理的低压撞击器收集的对应粒径段的灰颗粒作质量粒径分布的对比,或采用扫描电镜分析对应粒径段内灰胞颗粒的数目比例,验证粒径换算方法是否有效,对于有效的固体燃料样品进入第(5)步;(4) Compare the ash particles of each particle size segment identified in step (3) with the ash particles of the corresponding particle size segment collected by the low-pressure impactor based on the principle of aerodynamics for mass particle size distribution, or use scanning electron microscope analysis Corresponding to the number ratio of gray cell particles in the particle size segment, verify whether the particle size conversion method is valid, and enter step (5) for valid solid fuel samples;

(5)利用步骤(3)的统计结果对各粒径段的单颗粒进行物化性质分析,包括分析各粒径段颗粒物的矿物组成与含量;分析特定的矿物成分在各粒径段颗粒物中的赋存情况;分析主要成灰元素在颗粒物各粒径段、各矿物成分中的赋存情况。(5) Utilize the statistical results of step (3) to analyze the physicochemical properties of single particles in each particle size section, including analyzing the mineral composition and content of the particles in each particle size section; analyzing the specific mineral composition in the particles in each particle size section Occurrence: analyze the occurrence of main ash-forming elements in each particle size segment and mineral composition.

本发明针对灰分含Fe量低于5%的高阶煤或其它挥发分含量低于30%的固体燃料,收集燃烧后的灰样;通过粒径换算公式,将CCSEM分析所得灰样的几何粒径换算为空气动力学直径,实现颗粒物的识别,即识别出多个粒径段的颗粒物,如具有代表性的空气动力学直径0.5-10μm粒径段的PM0.5-10,以及PM0.5-2.5和PM2.5-10等;对PM0.5-10进行单颗粒分析,实现对各粒径段颗粒物的矿物组成,特定矿物成分在各粒径段颗粒物中赋存情况,主要成灰元素在颗粒物各粒径段、各矿物成分中赋存形态等分析。The present invention collects the ash samples after combustion for high-rank coals with an ash Fe content lower than 5% or other solid fuels with a volatile content lower than 30%; through the particle size conversion formula, the geometric particle size of the ash samples analyzed by CCSEM is The diameter is converted into the aerodynamic diameter to realize the identification of particulate matter, that is, to identify particulate matter with multiple particle size segments, such as PM 0.5-10 and PM 0.5-2.5 in the representative aerodynamic diameter range of 0.5-10 μm and PM 2.5-10 , etc.; perform single-particle analysis on PM 0.5-10 to realize the mineral composition of particles in each particle size segment, the occurrence of specific mineral components in particles in each particle size segment, and the main ash-forming elements in each particle size Diameter section, occurrence form of each mineral composition, etc.

总之,本发明借助CCSEM技术识别固体燃料燃烧后颗粒物与分析其物化性质,对燃烧生成的飞灰进行单颗粒分析,实现对PM0.5-10单颗粒的识别及物化特性的分析,充分了解固体燃料燃烧生成颗粒物统计学意义上的物化特征,为固体燃料颗粒物的来源、元素赋存形态等重要参数的建立与分析提供理论与技术指导。In a word, the present invention uses CCSEM technology to identify particulate matter after solid fuel combustion and analyze its physical and chemical properties, and conduct single particle analysis on fly ash generated by combustion, so as to realize the identification of PM 0.5-10 single particles and the analysis of physical and chemical characteristics, and fully understand the solid fuel Statistical physical and chemical characteristics of particulate matter generated by combustion provide theoretical and technical guidance for the establishment and analysis of important parameters such as the source of solid fuel particulate matter and the occurrence form of elements.

附图说明Description of drawings

图1为CCSEM识别与LPI收集的PM0.5-10质量粒径分布示意图;Figure 1 is a schematic diagram of the mass particle size distribution of PM 0.5-10 identified by CCSEM and collected by LPI;

图2为PM0.5-2.5、PM2.5-10和全灰各自的矿物组成示意图;Figure 2 is a schematic diagram of the respective mineral compositions of PM 0.5-2.5 , PM 2.5-10 and all ash;

图3为PM0.5-10及典型矿物成分在10μm内各粒径段质量分布示意图;Figure 3 is a schematic diagram of the mass distribution of PM 0.5-10 and typical mineral components in each particle size segment within 10 μm;

图4为Fe元素在灰(颗粒物)各矿物成分中的质量分布示意图。Fig. 4 is a schematic diagram of mass distribution of Fe element in various mineral components of ash (particulate matter).

具体实施方式Detailed ways

为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例对本发明进行详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,但本发明并不受此实施例的限制。In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiment described here is only used to explain the present invention, but the present invention is not limited by this embodiment.

本发明提供的一种对固体燃料燃烧后颗粒物单颗粒识别与分析的方法,其步骤包括:The invention provides a method for identifying and analyzing a single particle of particulate matter after solid fuel combustion, the steps of which include:

(1)收集固体燃料燃烧后的灰样,利用计算机控制扫描电镜(CCSEM)技术分析每个灰颗粒的几何粒径、元素成分、矿物种类与含量;(1) Collect ash samples after solid fuel combustion, and use computer-controlled scanning electron microscope (CCSEM) technology to analyze the geometric particle size, element composition, mineral type and content of each ash particle;

将飞灰与巴西棕榈蜡均匀混合后经熔融、冷却、研磨、抛光,制得分散度良好的样品,在环境扫描电镜中得到样品的背散射图像;选取足量的图像数目获取2000-3000个灰颗粒的数据,以满足统计学意义的分析;在能谱“Particles”功能中分析得到每个灰颗粒的几何粒径和无机元素组成;将每个灰颗粒按元素组成划分至具体的灰矿物种类,该种类所有颗粒的质量和即为该矿物成分在灰中的含量。Mix the fly ash and carnauba wax evenly, melt, cool, grind, and polish to obtain a sample with good dispersion, and obtain the backscattered image of the sample in an environmental scanning electron microscope; select a sufficient number of images to obtain 2000-3000 The data of ash particles to meet the analysis of statistical significance; analyze the geometric particle size and inorganic element composition of each ash particle in the "Particles" function of the energy spectrum; divide each ash particle into specific ash minerals according to the element composition type, the mass sum of all particles of this type is the content of the mineral component in the ash.

(2)利用步骤(1)的分析结果,采用几何粒径与空气动力学直径的换算公式将将每个灰颗粒的几何粒径换算为空气动力学直径;几何粒径d与空气动力学直径daer的换算公式为灰颗粒密度ρ取步骤(1)所定义矿物种类对应的密度值。(2) Utilize the analytical result of step (1), adopt the conversion formula of geometric particle diameter and aerodynamic diameter to convert the geometric particle diameter of each ash particle into aerodynamic diameter; Geometric particle diameter d and aerodynamic diameter The conversion formula of d aer is Ash particle density ρ takes the density value corresponding to the mineral type defined in step (1).

(3)利用步骤(2)可识别出各粒径段的颗粒物,如空气动力学直径0.5-10μm粒径段的颗粒物,记为PM0.5-10,以及多种典型粒径段的颗粒物,如PM0.5-2.5、PM2.5-10等。(3) Step (2) can be used to identify particles of various particle sizes, such as particles with an aerodynamic diameter of 0.5-10 μm, which are recorded as PM 0.5-10 , and particles of various typical particle sizes, such as PM 0.5-2.5 , PM 2.5-10 , etc.

应当说明的是,受扫描电镜的技术精度所限,目前无法实现0.5μm以内超细颗粒物的单颗粒分析。It should be noted that, limited by the technical precision of the scanning electron microscope, it is currently impossible to achieve single particle analysis of ultrafine particles within 0.5 μm.

(4)可采用两种方式证实粒径换算结果的有效性:一为采用基于空气动力学原理的LPI收集PM10,其与步骤(3)所识别的PM0.5-10作质量粒径分布的对比以验证CCSEM测试与颗粒粒径换算的有效性;二为观察扫描电镜形貌图中灰胞颗粒的存在情况,灰胞的存在会导致灰颗粒密度与换算公式输入值有差别。(4) Two methods can be used to verify the validity of the particle size conversion results: one is to use LPI based on aerodynamic principles to collect PM 10 , which is used as the mass particle size distribution of PM 0.5-10 identified in step (3). The comparison is to verify the validity of CCSEM test and particle size conversion; the second is to observe the existence of gray cells in the scanning electron microscope topography image, the existence of gray cells will cause the difference between the density of gray particles and the input value of the conversion formula.

“验证方式一”中质量粒径分布内每级颗粒物数据偏差小于20%时认为是有效验证;“验证方式二”观察形貌图后,灰胞颗粒数目占总灰颗粒比例低于10%时,认为是有效验证。多个数据测试结果表明,灰分含Fe量低于5%的烟煤、无烟煤等高阶煤,以及挥发分含量低于30%的其它固体燃料燃烧后产生较少的灰胞颗粒,且粒径换算结果与LPI测试结果基本吻合,因此适用于本换算公式。两种验证方式可以任选一种,验证后无效的固体燃料样品则认为不适用于此方法。In "Verification Method 1", when the deviation of each level of particle data in the mass particle size distribution is less than 20%, it is considered to be effective verification; in "Verification Method 2", after observing the topography, the number of gray cells accounts for less than 10% of the total gray particles , which is considered valid verification. The results of multiple data tests show that high-rank coals such as bituminous coal and anthracite with ash content less than 5% Fe, and other solid fuels with a volatile content less than 30% produce fewer ash cell particles after combustion, and the particle size conversion The results are basically consistent with the LPI test results, so it is suitable for this conversion formula. One of the two verification methods can be selected, and solid fuel samples that are invalid after verification are considered not applicable to this method.

(5)经步骤(4)验证后对PM0.5-10的单颗粒物化性质进行分析。基于步骤(1)-(3)识别每个灰颗粒的空气动力学直径及矿物种类、含量,汇总后可得到各粒径段颗粒物的矿物组成,如PM0.5-2.5和PM2.5-10各自的矿物种类与含量,以及某特定的矿物成分种类在各粒径段颗粒物中的赋存情况。基于步骤(1)识别每个灰颗粒的元素组成,计算某元素在该灰颗粒中的质量,汇总每个灰颗粒的空气动力学直径及矿物成分种类数据后,可分析主要成灰元素在颗粒物各粒径段、各矿物成分中的赋存情况。(5) Analyze the physical and chemical properties of single particles of PM 0.5-10 after step (4) verification. Based on steps (1)-(3) to identify the aerodynamic diameter, mineral type and content of each ash particle, the mineral composition of each particle size segment can be obtained after summarization, such as PM 0.5-2.5 and PM 2.5-10 respectively Mineral types and contents, as well as the occurrence of a specific type of mineral composition in the particles of each particle size. Based on step (1) to identify the element composition of each ash particle, calculate the mass of an element in the ash particle, and summarize the aerodynamic diameter and mineral composition data of each ash particle, the main ash-forming elements in the particle can be analyzed Occurrence in each particle size segment and mineral composition.

实例:Example:

本实施例所公开的对固体燃料燃烧后颗粒物单颗粒识别与分析的方法,具体步骤如下:The specific steps of the method for identifying and analyzing single particles of particulate matter after solid fuel combustion disclosed in this embodiment are as follows:

(1)本实施例所选燃料为一种典型的动力用煤:阳泉无烟煤,收集煤粉在实验室规模沉降炉中1300℃、空气气氛燃烧后的灰样。(1) The fuel selected in this example is a typical power coal: Yangquan anthracite, and the ash samples of pulverized coal burned in a laboratory-scale settling furnace at 1300°C in an air atmosphere were collected.

(2)利用CCSEM技术分析灰样,分析的具体方法为:在环境扫描电镜中得到飞灰样品清晰的背散射图像,获得每个灰颗粒的几何粒径;对灰颗粒进行能谱分析得到单颗粒的无机元素组成;在能谱“Particles”功能中选取足量的图像数目,以保证计算机对样品自动分析满足统计学计算意义的2000-3000个灰颗粒;将每个灰颗粒按各自的元素组成划分至具体的矿物种类;定义为同种矿物的所有灰颗粒质量加和即为该灰矿物成分的含量。(2) Using CCSEM technology to analyze the gray sample, the specific method of analysis is: obtain a clear backscattered image of the fly ash sample in the environmental scanning electron microscope, and obtain the geometric particle size of each ash particle; conduct energy spectrum analysis on the ash particle to obtain a single Inorganic element composition of particles; select a sufficient number of images in the "Particles" function of the energy spectrum to ensure that the automatic analysis of the sample by the computer meets the statistical calculation of 2000-3000 gray particles; The composition is divided into specific mineral types; defined as the sum of the mass of all ash particles of the same mineral is the content of the ash mineral composition.

(3)利用步骤(2)的分析结果,采用几何粒径d与空气动力学直径daer的换算公式将每个灰颗粒的几何粒径换算为空气动力学直径,灰颗粒密度ρ取步骤(2)所定义矿物的密度值,由此可识别出PM0.5-10(3) Utilize the analysis result of step (2), adopt the conversion formula of geometric particle diameter d and aerodynamic diameter d aer The geometric particle size of each ash particle is converted into an aerodynamic diameter, and the ash particle density ρ takes the density value of the mineral defined in step (2), so that PM 0.5-10 can be identified.

(4)采用LPI收集PM10,其与步骤(3)所识别的PM0.5-10作相同粒径范围内质量分数粒径分布的对比,如图1所示,两种方法收集的PM0.5-2.5粒径分布非常相似,2.5-10μm范围的颗粒物分布相差相对更大,可能是部分灰胞颗粒对换算公式准确性的影响;总体而言,该实例下两种方法得到的粒径分布吻合良好。扫描电镜形貌图也显示灰样中几乎不存在灰胞颗粒,对换算公式所采用的各灰矿物成分密度值影响很小。(4) Use LPI to collect PM 10 , and compare it with the PM 0.5-10 identified in step (3) in the mass fraction particle size distribution in the same particle size range, as shown in Figure 1, the PM 0.5-10 collected by the two methods 2.5 The particle size distribution is very similar, and the particle size distribution in the range of 2.5-10 μm is relatively different, which may be the influence of some gray cell particles on the accuracy of the conversion formula; overall, the particle size distribution obtained by the two methods in this example is in good agreement . The scanning electron microscope topography also shows that there are almost no gray cell particles in the gray sample, which has little effect on the density values of the various gray mineral components used in the conversion formula.

(5)利用步骤(1)-(3)识别PM0.5-10,并利用步骤(4)证实该粒径换算方法的有效性;随后对PM0.5-10的单颗粒物化特征进行具体分析。(5) Use steps (1)-(3) to identify PM 0.5-10 , and use step (4) to verify the effectiveness of the particle size conversion method; then analyze the physical and chemical characteristics of single particles of PM 0.5-10 .

图2分析各粒径段颗粒物的矿物组成,以PM0.5-2.5、PM2.5-10与全灰样为例,结果表明,PM0.5-2.5主要的灰矿物成分是Fe硅铝酸盐、混合硅铝酸盐和难识别成分,而PM2.5-10的主量矿物成分是莫来石和Fe硅铝酸盐。Figure 2 analyzes the mineral composition of particulate matter in each particle size range, taking PM 0.5-2.5 , PM 2.5-10 and the whole ash sample as examples, the results show that the main ash mineral components of PM 0.5-2.5 are Fe aluminosilicate, mixed silicon Aluminate and difficult to identify components, while the main mineral components of PM 2.5-10 are mullite and Fe aluminosilicate.

图3分析特定矿物成分在各粒径段颗粒物中的赋存情况,与PM0.5-10分布的比较可发现,Fe硅铝酸盐多富集在2.5μm颗粒以下,而莫来石相成分则多存在于2.5-10μm的较粗颗粒粒径段。Figure 3 analyzes the occurrence of specific mineral components in particles of various particle sizes. Compared with the distribution of PM 0.5-10 , it can be found that Fe aluminosilicates are mostly enriched below 2.5 μm particles, while the mullite phase components are It mostly exists in the coarse particle size section of 2.5-10μm.

图4分析成灰元素在颗粒物各粒径段、各矿物成分中的赋存情况,以Fe元素为例,Fe在PM0.5-2.5中多存在于Fe硅铝酸盐和难识别成分;PM2.5-10中的Fe分布在Fe硅铝酸盐、莫来石和难识别成分中的含量均较大。Figure 4 analyzes the occurrence of ash-forming elements in various particle sizes and mineral components. Taking Fe as an example, Fe mostly exists in Fe aluminosilicates and difficult-to-identify components in PM 0.5-2.5 ; PM 2.5 The content of Fe in -10 is relatively large in Fe aluminosilicate, mullite and difficult to identify components.

本发明不限于实施例的限制,同样适用于灰分含Fe量低于5%的煤种与挥发分含量低于30%的固体燃料。以上所述,仅为本发明的一种具体实施方式,但本发明保护的范围并不局限于此。任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。The present invention is not limited to the limitations of the examples, and is also applicable to coal types with an ash Fe content lower than 5% and solid fuels with a volatile matter content lower than 30%. The above description is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any person skilled in the art within the technical scope disclosed in the present invention shall fall within the protection scope of the present invention.

Claims (4)

1.一种对固体燃料颗粒物单颗粒识别与分析的方法,包括以下步骤:1. A method for solid fuel particulate single particle identification and analysis, comprising the following steps: (1)收集固体燃料燃烧后的灰样,利用计算机控制扫描电镜分析每个灰颗粒的几何粒径、元素成分、矿物种类与含量;(1) Collect the ash samples after solid fuel combustion, and analyze the geometric particle size, elemental composition, mineral type and content of each ash particle with a computer-controlled scanning electron microscope; (2)采用几何粒径与空气动力学直径的换算公式,将步骤(1)得到的每个灰颗粒的几何粒径换算为空气动力学直径;(2) adopt the conversion formula of geometric particle diameter and aerodynamic diameter, the geometric particle diameter of each ash particle that step (1) obtains is converted into aerodynamic diameter; (3)识别出空气动力学直径在各粒径段的灰颗粒;(3) Identify the ash particles whose aerodynamic diameter is in each particle size segment; (4)将步骤(3)识别出的各粒径段的灰颗粒与基于空气动力学原理的低压撞击器收集的对应粒径段的灰颗粒作质量粒径分布的对比,或采用扫描电镜分析对应粒径段内灰胞颗粒的数目比例,验证粒径换算方法是否有效,对于有效的固体燃料样品进入第(5)步;(4) Compare the ash particles of each particle size segment identified in step (3) with the ash particles of the corresponding particle size segment collected by an aerodynamic low-pressure impactor for mass particle size distribution, or use scanning electron microscope analysis Corresponding to the number ratio of gray cell particles in the particle size segment, verify whether the particle size conversion method is valid, and enter step (5) for valid solid fuel samples; (5)利用步骤(3)的统计结果对各粒径段的单颗粒进行物化性质分析,包括分析各粒径段颗粒物的矿物组成与含量;分析特定的矿物成分在各粒径段颗粒物中的赋存情况;分析主要成灰元素在颗粒物各粒径段、各矿物成分中的赋存情况。(5) Utilize the statistical results of step (3) to analyze the physicochemical properties of single particles in each particle size section, including analyzing the mineral composition and content of the particles in each particle size section; analyzing the specific mineral composition in the particles in each particle size section Occurrence: analyze the occurrence of main ash-forming elements in each particle size segment and mineral composition. 2.根据权利要求1所述的方法,其特征在于,所述利用计算机控制扫描电镜分析灰颗粒的方法如下:将飞灰与巴西棕榈蜡均匀混合制得样品,在扫描电镜中得到飞灰背散射图像;选取足量的图像数目以获取满足统计学分析的2000-3000个灰颗粒,再分析每个灰颗粒的几何粒径和元素组成。2. The method according to claim 1, characterized in that, the method for analyzing ash particles by computer-controlled scanning electron microscope is as follows: fly ash and carnauba wax are uniformly mixed to obtain a sample, and the fly ash back is obtained in a scanning electron microscope. Scattering images: select enough images to obtain 2000-3000 gray particles that satisfy the statistical analysis, and then analyze the geometric particle size and elemental composition of each gray particle. 3.根据权利要求1所述的方法,其特征在于:用于对包括PM0.5-2.5、PM2.5-10和PM0.5-10在内的任一或任几个粒径段的颗粒物分别进行统计与分析。3. The method according to claim 1, characterized in that it is used to count the particulate matter of any or any number of particle size segments including PM 0.5-2.5 , PM 2.5-10 and PM 0.5-10 and analyse. 4.根据权利要求1所述的方法,其特征在于:适用燃料为灰分含Fe量低于5%的烟煤、无烟煤及其它挥发分含量低于30%的固体燃料。4. The method according to claim 1, characterized in that: the applicable fuel is bituminous coal, anthracite and other solid fuels with a volatile matter content lower than 30% with an ash content of Fe less than 5%.
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