加压流化床气化条件下灰熔融特性研究
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摘要
灰熔融性是煤及生物质燃烧和气化过程的一项重要性质。在流化床燃烧气化系统中,灰熔融特性对床料团聚、换热器积灰和管壁结渣等一系列现象有决定影响,并直接决定着排渣方式的选择,是影响煤及生物质燃烧和气化过程的一个重要因素。为研究灰熔融特性对加压流化床燃烧和气化系统的影响,利用自主研发的加压压差法烧结温度测量装置、加压热天平装置和灰熔点仪等装置,结合热力学软件FactSage、X射线衍射分析仪以及扫描电镜和能量色散荧光分析仪,对煤及其与生物质混合燃料的灰熔融特性开展了系统的分析研究。主要系统考察了加压燃烧气化过程中化学组分、温度、气氛和压力等因素对灰熔融特性的影响特性及灰中矿物质组分的转变特性,并利用相图理论,将不同温度和压力下的矿物质转变直观地用相图表示出来,探讨了加压流化床气化条件下的灰熔融机理。主要的研究工作及结果如下：
(1)利用所建的加压压差法烧结温度测量装置结合X射线衍射分析仪,研究了反应气氛、压力及灰组分对煤灰烧结温度的影响特性及其机理。结果表明无论是常压还是加压条件,在还原性气氛下的煤灰烧结温度都低于氧化性气氛下煤灰的烧结温度,主要原因是在还原性气氛下,部分Fe3+转化为Fe2+后,易和灰中其他组分如含钙、钠等化合物反应生成易于发生低温共融的矿物质,如铁橄榄石与铁尖晶石等,导致烧结温度降低。压力对煤灰的烧结温度有较大的影响,压力的升高抑制硬石膏、钾云母等助融矿物质分解,与微斜长石、赤铁矿、钙长石等矿物组分共存,发生低温共融现象,从而使得烧结温度下降。燃烧和气化气氛下,在煤灰中添加CaO、Fe2O3和Na2O都会降低煤灰烧结温度,其中CaO和Na2O含量对煤灰烧结温度影响较大。其主要原因是Fe2O3、CaO和Na2O等氧化物将促使一些低温易熔矿物质或易与其他矿物质形成低温共融体的矿物质形成,如无水芒硝、钙长石、钠长石等长石类矿物质,以及铁尖晶石、铁橄榄石、铁堇青石等铁系矿物质(气化气氛下)。
同时,利用压差法烧结温度测量装置,对加压条件下不同混合比例的煤和生物质混合灰进行了烧结特性的研究,同时还测量了山西晋城煤与麦秆/松木屑的混合灰样的烧结温度。结合SEM-EDS及XRD分析方法,分析了烧结样品的形貌特征、元素组成及其中的矿物质组成。结果表明：随着麦秆比例的增加,灰样的烧结温度也呈现降低趋势,且降低幅度较大。随着麦秆比例的添加,灰样呈现明显团聚和烧结现象,且灰样中K、Cl的含量显著增加,而麦秆灰中还有较高含量的碱金属,会生成较多的含钾、钠的低熔点的矿物质,这是导致烧结温度降低的主要原因。而在掺混同样的生物质比例时,掺混麦秆的混合灰样的烧结温度低于掺混木屑的灰样的烧结温度,这是因为麦秆灰中含有较多的K和Cl,而木屑灰中含有较多的Ca。EDS和XRD分析表明添加麦秆的灰样中含有较多的含钾矿物,而添加木屑的灰样中含有较多的含钾和钙的矿物质,含钾、钙的矿物质都能与煤中其他矿物质发生低温共融现象,从而降低混合灰样的烧结温度。但是含钙的矿物的熔点较高,因此添加麦秆的灰样的烧结温度低于添加木屑的灰样的烧结温度。随着压力升高,燃烧气氛和气化气氛下添加不同生物质比例的灰样的烧结温度呈现明显下降趋势。压力升高导致灰样更加致密,这说明压力升高导致更多的助融矿物发生熔融,从而使得熔融聚团现象更加严重。压力升高,促使添加了生物质的混合灰样中透辉石、钙黄长石向含铁矿物质斜晖石的转变,长石类矿物质钙长石的生成。而长石类矿物质和含铁矿物质及易与其他矿物质发生低温共熔现象,促使烧结温度降低。
最后,为研究成灰过程的影响,选用山西晋城煤和澳大利亚的麦秆和松木屑为原料,采用高温直管式炉、中温马弗炉、低温氧等离子体灰化仪三种不同的灰化方法制备灰样。利用压差法烧结温度测量装置测量了混合灰样的烧结温度,并采用SEM-EDS和XRD分析仪分析了混合灰样的形貌特征及矿物转变特性。研究结果表明：同样的煤和生物质的混合比例下,直管式炉中混合灰样的烧结温度最高,低温等离子体灰化仪中混合灰样的烧结温度最低。SEM分析表明来自低温等离子体灰化仪中的灰样颗粒比较疏松且含有更多的纤维结构；而马弗炉和直管式炉中的灰样表面结构比较致密,并成规则的形状。此外,来自直管式炉的灰样中出现较多球状颗粒,表明在灰样过程中发生了熔融现象。XRD分析表明不同温度下的灰样制备方式呈现不同的矿物质,低温等离子体灰化仪中出现较低温度的矿物质如钾芒硝等,马弗炉中出现KCl和钾云母等助融矿物质,而直管式炉中出现如钙长石、莫来石等较高温度的矿物质。
(2)利用加压热天平结合XRD分析仪及SEM-EDS分析仪,开展了加压流化床燃烧气化条件下压力、气氛、温度和灰成分影响煤灰矿物质的转变过程的实验研究。研究结果表明不同反应气氛下压力对煤灰中矿物质的转化过程具有明显不同的影响。在气化气氛下,压力的升高促使陨硫钙石向硬石膏的转变,抑制钾云母、硬石膏等助融矿物质分解,促使长石类矿物质透长石生成和铁系矿物质赤铁矿熔融；而在惰性气氛和燃烧气氛下,压力的变化促使钾云母向莫来石转变,而微斜长石向钠长石转变,而对其他矿物质影响不大。随着温度逐渐升高,在气化气氛下,生成钙长石相及铁尖晶石等矿物相,而他们会与其他矿物质发生低温共熔现象,从而降低灰熔融温度；在燃烧气氛下,随着温度升高,生成透长石等长石类矿物质和莫来石等高熔点矿物质,升高灰熔融温度。随着Fe2O3含量增加,燃烧气氛下煤灰中生成了磁铁矿、硬石膏、钾云母以及微斜长石等助融矿物质；气化气氛下生成了铁尖晶石、钠长石等易与其他矿物发生低温共融的矿物质。而随着CaO的增加,燃烧气氛下生成钾云母、硬石膏等助融矿物质及方解石和钙黄长石等易与发生低温共融的矿物质；在气化气氛下除了钾云母、钙黄长石和方解石外,还生成了钙长石等易形成低温共融体的矿物质。随着Na2O含量的增加,燃烧气氛下出现钾云母、硬石膏和赤铁矿和霞石等助融矿物质；在气化气氛下发生了铁尖晶石的熔融,并出现了霞石等助融矿物质及钙黄长石等易发生低温共融的矿物质。
(3)利用灰熔点仪,测定了不同气氛下、不同灰成分下的灰熔融温度,并结合FactSage软件模拟计算结果分析了气氛和灰组分对灰熔融温度的影响特性,结果表明：随着Fe2O3、CaO及Na2O的增加,在燃烧和气化气氛下变形温度、软化温度、半球温度和流动温度等特征温度都呈现降低趋势；随着Fe2O3、CaO及Na2O这三种氧化物含量的增加,煤灰中的矿物质在不同气氛下发生相变反应并伴随新的矿物质的生成。随着Fe2O3含量的增加,煤灰中出现铁系矿物质,如磁铁矿、铁尖晶石和铁橄榄石等；随着CaO的增加,出现含钙的长石类矿物质钙黄长石等；随着Na2O含量的增加,促进三斜霞石等含钠的长石类矿物质等的生成。所生成的铁系矿物质、含钙及钠的长石类矿物质中,有一些是本身熔点较低,有一些是易与其他矿物质形成低温共融体,这些矿物质的存在是煤灰熔融温度降低的根本原因。
(4)在实验研究基础上,利用相图理论将不同温度、压力段下的矿物成分分布整理成相图,直观地呈现出不同温度带和不同压力下的矿物质,并利用三元相图理论分析了晋城煤灰的灰熔融特性。结果表明温度对矿物质转化过程影响较大,而压力对矿物转变影响相对较小。同时温度和压力的影响也与反应气氛有关。燃烧气氛下矿物物相种类变化较少,即燃烧气氛下矿物物相间发生的反应较少,而气化气氛下矿物种类变化较多,其发生物相转变较多。随着温度升高,在还原性气氛下促进Fe2+生成,煤灰中的含Fe2+的矿物质,通过与SiO2、Al2O3等化合物反应生成铁尖晶石等铁系矿物质相,在氧化气氛下硅铝酸盐则通过与碱金属化合物和碱土金属化合物反应生成长石类矿物质相,如钙长石,斜长石等。一般来说,长石类及铁系矿物质都会与其他矿物质如Na2O·2SiO2、K2O-4SiO2等发生低温共融现象,生成低温共融体如Na2O·2SiO2+SiO2+Na2O·3CaO·6SiO2等。随着压力升高,在惰性气氛、氧化性气氛下对矿物质生成种类影响不大,但压力升高促进结晶矿物质析出,对矿物质生成量有一定影响,同时受抑制分解的多种低温矿物质如钾云母、硬石膏等共存,会产生低温共融现象。在气化气氛下,压力升高促进硅铝酸盐与灰中碱金属化合物和碱土金属化合物反应,生成长石类矿物质如钙长石、透长石等,而长石类矿物质会产生低温共融现象。
The ash fusibility is an important factor in the coal and biomass combustion and gasification system. The effect of ash fusion characteristics on the bed agglomeration, deposition on gas circuits and heat exchanger tubes is significant during the combustion and gasification process. The ash fusibility determines how to remove slags and influences the combustion and gasification process of coal and biomass. In order to investigate the effect of ash fusion behavior on the pressurized fluidized bed combustion and gasification system, we used the pressurized pressure-drop measuring device, high pressure TGA and ash fusion determinator, together with thermodynamic software FactSage, X-ray diffraction analyzer (XRD) and scanning electron microscopy fitted with X-ray energy dispersive spectroscopy (SEM-EDS) and studied the ash fusion behavior of coal and biomass systematically. The effects of ash composition, temperatures, reaction atmospheres and pressures on the ash fusibility, as well as the mineral transformation characteristics, were investigated. Finally, we employed the phase theory to investigate the ash fusibility mechanism during the pressurized fluidized bed combustion and gasification, based on the experimental results. The main contents are listed as follows:
(1) The effects of different atmospheres, pressures and ash composition on the sintering temperature were studied using the pressurized pressure-drop device, together with XRD analyzer. The results showed that the sintering temperatures under the reducing atmosphere were lower than those of oxidizing atmosphere. Under a reducing atmosphere, some Fe3+would be converted to Fe2+at higher temperature, and Fe2+reacted with other ash constituents to form fayalite, hercynite, etc., which can form the low temperature eutectics and decreased the sintering temperature. Pressure had big influences on the sintering temperatures. This was because the pressure affects the transformaions of minerals during heating and facilitates the form of fluxing minerals such as anhydrite, microcline and hematite etc. and minerals like anorthite which can react with other minerals to form low-temperature eutectics, leading to the reduction of sintering temperatures. The additives of CaO, Fe2O3and Na2O reduced the sintering temperatures under the combustion and gasification atmospheres during atmospheric and high pressure. Moreovver, the influences of CaO and Na2O on the sintering temperature were more significant than that of Fe2O3. With the increases in CaO, Fe2O3and Na2O, some fluxing minerals and low temperature eutectics were formed in the coal ash, such Na2SO4, anorthite, albite and iron-bearing minerals like hercynite and fayalite etc (in the gasification atmosphere). These minerals reacted with other minerals to form the low temperature eutectics, leading to the reduction of the sintering temperature.
Secondly, the ash sintering behavior of the coal and biomass was studied using the pressurized pressure-drop device, together with SEM-EDS and XRD analyzer. The results showed that the sintering temperatures of ash samples decreased with the additive of biomass under the combustion and gasification atmospheres, the higher the proportion of biomass addition in the blend, the lower the ash sintering temperature. SEM-EDS results showed that agglomeration and sintering were detected in the ash samples and the content of K and Cl increased obviously with the addition of straw. High contents of alkali metal like K and Na facilitated the form of K and Na-containing minerals, which have low melting points. This is the main reason resulting in the decrease of sintering temperature. At the same blending ratio, the ash sintering temperature of the blend with the straw addition was lower than that with the sawdust addition, because the straw had a higher K and Cl content but lower Ca than the sawdust. The EDS and XRD analysis confirmed that the ash samples with straw addition contained more K-bearing minerals, while the ash samples with sawdust contained more Ca and K-bearing minerals. Both Ca and K-bearing minerals reacted with other minerals in the coal to form low temperature eutectics, leading to the reduction of sintering temperatures of the coal and biomass blends. However, the melting point of Ca-containing is higher than the K-containing minerals, therefore, the sintering temperatures of ash with straw addition were lower than those with sawdust addition. The sintering temperatures decreased with the increase in pressure. As the pressure increased, the ash with the addition of biomass showed denser in the texture. This indicated that more fluxing minerals melted with increasing the pressure, and thereby leading to the agglomeration singnificantly. XRD analysis showed that the pressure facilitated the transformations of diopside and gelhcnite into augite and anorthite. The iron-bearing mineral augite and feldspar mineral anorthite can reacted with other minerals to form the low temperature eutectics, leading to the decrease of the sintering temperature.
Finally, blends of Jincheng coal, and a wheat straw and a pine sawdust, respectively, were subjected to three different ash preparation procedures, namely, a low temperature oxygen plasma ashing device, muffle furnace and drop tube furnace. The resulting ash samples were then subjected to the sintering temperature measurement using a pressure-drop sintering device, morphological and mineralogical characterisation using SEM-EDS and XRD, respectively. For the same coal/biomass blends but different ash preparation methods, the sintering temperatures were always the lowest for the ash samples from the plasma ashing device and the highest for the drop tube furnace, with the muffle furnace ash samples being in between. The SEM imaging showed that the texture of ash samples from plasma ashing device was irregular, loose and more fibrous but the muffle furnace and drop tube furnace ashes were denser and more uniform in shape. In addition, the drop tube furnace ash particles were mostly in spherical-shape, indicating ash melting had occurred in the drop tube furnace. The XRD analysis revealed that different minerals were present in the ash samples due to different ash preparation temperatures. The minerals of the ash from the plasma ashing device were the low-temperature minerals, like aphthitalite. The fluxing minerals, such as KCl and muscovite, were present in the Muffle furnace ash and the high temperature minerals, such as anorthite and mullite were present in the drop tube furnace ash.
(2) A high pressure thennogravimetric analyzer, aided with X-ray diffraction (XRD) analyses and SEM-EDS analyses, were used to investigate the effects of reaction atmospheres, temperatures, pressures and ash composition on the mineralogical transformation of coal ash during pressurized fluidized bed combustion and gasification. The results showed that the pressure had obvious influences on the transformation of mineral under different reaction atmosphere. The pressure facilitated the transformations of oldhamite into anhydrite and the fusion of hematite and suppressed the decomposition of the fluxing minerals like muscovite and anhydrite under the gasification atmosphere. The influence of pressure on the mineral types was not obvious but only facilitated the transformations of the muscovite and microcline into mullite and the albite under the inertia and combustion atmospheres. The effect of temperature on the ash fusion characteristics was strongly dependent on the atmospheres. In gasification atmospheres, the iron-bearing minerals and feldspar minerals, such as hercynite and anorthite, became abundant and reacted with other minerals to form low-temperature eutectics, thus decreasing the fusion temperatures. In combustion atmospheres, more high temperature minerals such as sanidine and mullite were formed and dominate, leading to increases in the fusion temperatures. With the increase in Fe2O3, there were muscovite, magnetite and anhydrite, etc. in the combustion atmosphere, resulting in the decrease of the fusion temperature. In the gasification atmosphere, hercynite and albite were detected, which can react with other minerals to form low temperature eutectics. With increasing the CaO, there were the fluxing minerals (anhydrite, and hematite) and some feldspar minerals, such as calcite and gehlenite, easy to produce low-temperature eutectics with other minerals, and hereby declining the fusion temperature in the combustion atmosperes. In the gasification atmosphere, the anorthite was present along with anhydrite, hematite, calcite and gehlenite. With the increase in Na2O, there were fluxing minerals, such as muscovite, magnetite, anhydrite and nepheline in the combustion atmosphere; there were the fluxing minerals like nepheline and the minerals, like gehlenite, easy to produce low-temperature eutectics with other minerals, leading to the reduction of the fusion temperature.
(3) AFTs were examined under different atmospheres and ash composition using ash fusion determinator. The effects of chemical components of ash and reaction atmospheres on the ash fusion behaviors have been analyzed under typical gasification and combustion atmospheres, aided with the FactSage software. The results indicated that with increasing the Fe2O3,CaO and Na20contents under the combustion and gasification atmospheres, the four temperatures DT, ST, HT and FT declined dramatically. With the increase in Fe2O3, CaO and Na2O contents, the generation and transformation of minerals occurred. The iron-containing minerals, such as hercynite and fayalite, were formed as increased the content of Fe2O3; the Ca-bearing feldspar minerals, like anorthite and gehlenite, were present with increasing the CaO content; and the Na-containing feldspar minerals, like carnegiete etc., were detected as the Na2O was increased. These three minerals can form low temperature eutectics, decreasing the fusion temperature.
(4) Based on the experimental results, the mineral distributions under different temperatures and pressures were displayed using the phase theory. The mechanism of ash fusion was analyzed using the phase theory. The effect of temperature on the mineral transformations was significant while the effect of pressure was not obvious. Meanwhile the atmospheres which the minerals were in were related to the effects of temperature and pressure. The transformations of minerals under gasification atmosphere were more than under the combustion atmosphere.
This indicated that more phase transformations occurred under the gasification atmosphere than the combustion atmosphere. With increasing the temperature, the Fe2+-bearing minerals, like hercynite, reacted with SiO2, Al2O3in ash to form iron-containing minerals like hercynite and fayalite etc. under the reducing atmosphere. The feldspar minerals, such as anorthite and microcline, were formed by the reactions between the alkali and alkali earth oxides and the SiO2Al2O3in the oxidizing atmosphere. In general, the feldspar minerals and the iron-bearing minerals can react with other minerals, such as Na2O·2SiO2、K2O·4SiO2, to form low temperature eutectics like Na2O·2SiO2+SiO2+Na2O·3CaO·6SiO2. With the increase in pressure, the mineral transformations are not obvious in the oxidizing and inert atmospheres, however, the pressure affects the crystallization of minerals. Moreover, the fluxing minerals like muscovite and anhydrite coexisted and produced low temperature melting. Pressure facilitated the form of the feldspar minerals, like anorthite, sanidine etc. in the gasification atmosphere. The feldspar minerals can form the low temperature eutectics.
(1)利用所建的加压压差法烧结温度测量装置结合X射线衍射分析仪,研究了反应气氛、压力及灰组分对煤灰烧结温度的影响特性及其机理。结果表明无论是常压还是加压条件,在还原性气氛下的煤灰烧结温度都低于氧化性气氛下煤灰的烧结温度,主要原因是在还原性气氛下,部分Fe3+转化为Fe2+后,易和灰中其他组分如含钙、钠等化合物反应生成易于发生低温共融的矿物质,如铁橄榄石与铁尖晶石等,导致烧结温度降低。压力对煤灰的烧结温度有较大的影响,压力的升高抑制硬石膏、钾云母等助融矿物质分解,与微斜长石、赤铁矿、钙长石等矿物组分共存,发生低温共融现象,从而使得烧结温度下降。燃烧和气化气氛下,在煤灰中添加CaO、Fe2O3和Na2O都会降低煤灰烧结温度,其中CaO和Na2O含量对煤灰烧结温度影响较大。其主要原因是Fe2O3、CaO和Na2O等氧化物将促使一些低温易熔矿物质或易与其他矿物质形成低温共融体的矿物质形成,如无水芒硝、钙长石、钠长石等长石类矿物质,以及铁尖晶石、铁橄榄石、铁堇青石等铁系矿物质(气化气氛下)。
同时,利用压差法烧结温度测量装置,对加压条件下不同混合比例的煤和生物质混合灰进行了烧结特性的研究,同时还测量了山西晋城煤与麦秆/松木屑的混合灰样的烧结温度。结合SEM-EDS及XRD分析方法,分析了烧结样品的形貌特征、元素组成及其中的矿物质组成。结果表明：随着麦秆比例的增加,灰样的烧结温度也呈现降低趋势,且降低幅度较大。随着麦秆比例的添加,灰样呈现明显团聚和烧结现象,且灰样中K、Cl的含量显著增加,而麦秆灰中还有较高含量的碱金属,会生成较多的含钾、钠的低熔点的矿物质,这是导致烧结温度降低的主要原因。而在掺混同样的生物质比例时,掺混麦秆的混合灰样的烧结温度低于掺混木屑的灰样的烧结温度,这是因为麦秆灰中含有较多的K和Cl,而木屑灰中含有较多的Ca。EDS和XRD分析表明添加麦秆的灰样中含有较多的含钾矿物,而添加木屑的灰样中含有较多的含钾和钙的矿物质,含钾、钙的矿物质都能与煤中其他矿物质发生低温共融现象,从而降低混合灰样的烧结温度。但是含钙的矿物的熔点较高,因此添加麦秆的灰样的烧结温度低于添加木屑的灰样的烧结温度。随着压力升高,燃烧气氛和气化气氛下添加不同生物质比例的灰样的烧结温度呈现明显下降趋势。压力升高导致灰样更加致密,这说明压力升高导致更多的助融矿物发生熔融,从而使得熔融聚团现象更加严重。压力升高,促使添加了生物质的混合灰样中透辉石、钙黄长石向含铁矿物质斜晖石的转变,长石类矿物质钙长石的生成。而长石类矿物质和含铁矿物质及易与其他矿物质发生低温共熔现象,促使烧结温度降低。
最后,为研究成灰过程的影响,选用山西晋城煤和澳大利亚的麦秆和松木屑为原料,采用高温直管式炉、中温马弗炉、低温氧等离子体灰化仪三种不同的灰化方法制备灰样。利用压差法烧结温度测量装置测量了混合灰样的烧结温度,并采用SEM-EDS和XRD分析仪分析了混合灰样的形貌特征及矿物转变特性。研究结果表明：同样的煤和生物质的混合比例下,直管式炉中混合灰样的烧结温度最高,低温等离子体灰化仪中混合灰样的烧结温度最低。SEM分析表明来自低温等离子体灰化仪中的灰样颗粒比较疏松且含有更多的纤维结构；而马弗炉和直管式炉中的灰样表面结构比较致密,并成规则的形状。此外,来自直管式炉的灰样中出现较多球状颗粒,表明在灰样过程中发生了熔融现象。XRD分析表明不同温度下的灰样制备方式呈现不同的矿物质,低温等离子体灰化仪中出现较低温度的矿物质如钾芒硝等,马弗炉中出现KCl和钾云母等助融矿物质,而直管式炉中出现如钙长石、莫来石等较高温度的矿物质。
(2)利用加压热天平结合XRD分析仪及SEM-EDS分析仪,开展了加压流化床燃烧气化条件下压力、气氛、温度和灰成分影响煤灰矿物质的转变过程的实验研究。研究结果表明不同反应气氛下压力对煤灰中矿物质的转化过程具有明显不同的影响。在气化气氛下,压力的升高促使陨硫钙石向硬石膏的转变,抑制钾云母、硬石膏等助融矿物质分解,促使长石类矿物质透长石生成和铁系矿物质赤铁矿熔融；而在惰性气氛和燃烧气氛下,压力的变化促使钾云母向莫来石转变,而微斜长石向钠长石转变,而对其他矿物质影响不大。随着温度逐渐升高,在气化气氛下,生成钙长石相及铁尖晶石等矿物相,而他们会与其他矿物质发生低温共熔现象,从而降低灰熔融温度；在燃烧气氛下,随着温度升高,生成透长石等长石类矿物质和莫来石等高熔点矿物质,升高灰熔融温度。随着Fe2O3含量增加,燃烧气氛下煤灰中生成了磁铁矿、硬石膏、钾云母以及微斜长石等助融矿物质；气化气氛下生成了铁尖晶石、钠长石等易与其他矿物发生低温共融的矿物质。而随着CaO的增加,燃烧气氛下生成钾云母、硬石膏等助融矿物质及方解石和钙黄长石等易与发生低温共融的矿物质；在气化气氛下除了钾云母、钙黄长石和方解石外,还生成了钙长石等易形成低温共融体的矿物质。随着Na2O含量的增加,燃烧气氛下出现钾云母、硬石膏和赤铁矿和霞石等助融矿物质；在气化气氛下发生了铁尖晶石的熔融,并出现了霞石等助融矿物质及钙黄长石等易发生低温共融的矿物质。
(3)利用灰熔点仪,测定了不同气氛下、不同灰成分下的灰熔融温度,并结合FactSage软件模拟计算结果分析了气氛和灰组分对灰熔融温度的影响特性,结果表明：随着Fe2O3、CaO及Na2O的增加,在燃烧和气化气氛下变形温度、软化温度、半球温度和流动温度等特征温度都呈现降低趋势；随着Fe2O3、CaO及Na2O这三种氧化物含量的增加,煤灰中的矿物质在不同气氛下发生相变反应并伴随新的矿物质的生成。随着Fe2O3含量的增加,煤灰中出现铁系矿物质,如磁铁矿、铁尖晶石和铁橄榄石等；随着CaO的增加,出现含钙的长石类矿物质钙黄长石等；随着Na2O含量的增加,促进三斜霞石等含钠的长石类矿物质等的生成。所生成的铁系矿物质、含钙及钠的长石类矿物质中,有一些是本身熔点较低,有一些是易与其他矿物质形成低温共融体,这些矿物质的存在是煤灰熔融温度降低的根本原因。
(4)在实验研究基础上,利用相图理论将不同温度、压力段下的矿物成分分布整理成相图,直观地呈现出不同温度带和不同压力下的矿物质,并利用三元相图理论分析了晋城煤灰的灰熔融特性。结果表明温度对矿物质转化过程影响较大,而压力对矿物转变影响相对较小。同时温度和压力的影响也与反应气氛有关。燃烧气氛下矿物物相种类变化较少,即燃烧气氛下矿物物相间发生的反应较少,而气化气氛下矿物种类变化较多,其发生物相转变较多。随着温度升高,在还原性气氛下促进Fe2+生成,煤灰中的含Fe2+的矿物质,通过与SiO2、Al2O3等化合物反应生成铁尖晶石等铁系矿物质相,在氧化气氛下硅铝酸盐则通过与碱金属化合物和碱土金属化合物反应生成长石类矿物质相,如钙长石,斜长石等。一般来说,长石类及铁系矿物质都会与其他矿物质如Na2O·2SiO2、K2O-4SiO2等发生低温共融现象,生成低温共融体如Na2O·2SiO2+SiO2+Na2O·3CaO·6SiO2等。随着压力升高,在惰性气氛、氧化性气氛下对矿物质生成种类影响不大,但压力升高促进结晶矿物质析出,对矿物质生成量有一定影响,同时受抑制分解的多种低温矿物质如钾云母、硬石膏等共存,会产生低温共融现象。在气化气氛下,压力升高促进硅铝酸盐与灰中碱金属化合物和碱土金属化合物反应,生成长石类矿物质如钙长石、透长石等,而长石类矿物质会产生低温共融现象。
The ash fusibility is an important factor in the coal and biomass combustion and gasification system. The effect of ash fusion characteristics on the bed agglomeration, deposition on gas circuits and heat exchanger tubes is significant during the combustion and gasification process. The ash fusibility determines how to remove slags and influences the combustion and gasification process of coal and biomass. In order to investigate the effect of ash fusion behavior on the pressurized fluidized bed combustion and gasification system, we used the pressurized pressure-drop measuring device, high pressure TGA and ash fusion determinator, together with thermodynamic software FactSage, X-ray diffraction analyzer (XRD) and scanning electron microscopy fitted with X-ray energy dispersive spectroscopy (SEM-EDS) and studied the ash fusion behavior of coal and biomass systematically. The effects of ash composition, temperatures, reaction atmospheres and pressures on the ash fusibility, as well as the mineral transformation characteristics, were investigated. Finally, we employed the phase theory to investigate the ash fusibility mechanism during the pressurized fluidized bed combustion and gasification, based on the experimental results. The main contents are listed as follows:
(1) The effects of different atmospheres, pressures and ash composition on the sintering temperature were studied using the pressurized pressure-drop device, together with XRD analyzer. The results showed that the sintering temperatures under the reducing atmosphere were lower than those of oxidizing atmosphere. Under a reducing atmosphere, some Fe3+would be converted to Fe2+at higher temperature, and Fe2+reacted with other ash constituents to form fayalite, hercynite, etc., which can form the low temperature eutectics and decreased the sintering temperature. Pressure had big influences on the sintering temperatures. This was because the pressure affects the transformaions of minerals during heating and facilitates the form of fluxing minerals such as anhydrite, microcline and hematite etc. and minerals like anorthite which can react with other minerals to form low-temperature eutectics, leading to the reduction of sintering temperatures. The additives of CaO, Fe2O3and Na2O reduced the sintering temperatures under the combustion and gasification atmospheres during atmospheric and high pressure. Moreovver, the influences of CaO and Na2O on the sintering temperature were more significant than that of Fe2O3. With the increases in CaO, Fe2O3and Na2O, some fluxing minerals and low temperature eutectics were formed in the coal ash, such Na2SO4, anorthite, albite and iron-bearing minerals like hercynite and fayalite etc (in the gasification atmosphere). These minerals reacted with other minerals to form the low temperature eutectics, leading to the reduction of the sintering temperature.
Secondly, the ash sintering behavior of the coal and biomass was studied using the pressurized pressure-drop device, together with SEM-EDS and XRD analyzer. The results showed that the sintering temperatures of ash samples decreased with the additive of biomass under the combustion and gasification atmospheres, the higher the proportion of biomass addition in the blend, the lower the ash sintering temperature. SEM-EDS results showed that agglomeration and sintering were detected in the ash samples and the content of K and Cl increased obviously with the addition of straw. High contents of alkali metal like K and Na facilitated the form of K and Na-containing minerals, which have low melting points. This is the main reason resulting in the decrease of sintering temperature. At the same blending ratio, the ash sintering temperature of the blend with the straw addition was lower than that with the sawdust addition, because the straw had a higher K and Cl content but lower Ca than the sawdust. The EDS and XRD analysis confirmed that the ash samples with straw addition contained more K-bearing minerals, while the ash samples with sawdust contained more Ca and K-bearing minerals. Both Ca and K-bearing minerals reacted with other minerals in the coal to form low temperature eutectics, leading to the reduction of sintering temperatures of the coal and biomass blends. However, the melting point of Ca-containing is higher than the K-containing minerals, therefore, the sintering temperatures of ash with straw addition were lower than those with sawdust addition. The sintering temperatures decreased with the increase in pressure. As the pressure increased, the ash with the addition of biomass showed denser in the texture. This indicated that more fluxing minerals melted with increasing the pressure, and thereby leading to the agglomeration singnificantly. XRD analysis showed that the pressure facilitated the transformations of diopside and gelhcnite into augite and anorthite. The iron-bearing mineral augite and feldspar mineral anorthite can reacted with other minerals to form the low temperature eutectics, leading to the decrease of the sintering temperature.
Finally, blends of Jincheng coal, and a wheat straw and a pine sawdust, respectively, were subjected to three different ash preparation procedures, namely, a low temperature oxygen plasma ashing device, muffle furnace and drop tube furnace. The resulting ash samples were then subjected to the sintering temperature measurement using a pressure-drop sintering device, morphological and mineralogical characterisation using SEM-EDS and XRD, respectively. For the same coal/biomass blends but different ash preparation methods, the sintering temperatures were always the lowest for the ash samples from the plasma ashing device and the highest for the drop tube furnace, with the muffle furnace ash samples being in between. The SEM imaging showed that the texture of ash samples from plasma ashing device was irregular, loose and more fibrous but the muffle furnace and drop tube furnace ashes were denser and more uniform in shape. In addition, the drop tube furnace ash particles were mostly in spherical-shape, indicating ash melting had occurred in the drop tube furnace. The XRD analysis revealed that different minerals were present in the ash samples due to different ash preparation temperatures. The minerals of the ash from the plasma ashing device were the low-temperature minerals, like aphthitalite. The fluxing minerals, such as KCl and muscovite, were present in the Muffle furnace ash and the high temperature minerals, such as anorthite and mullite were present in the drop tube furnace ash.
(2) A high pressure thennogravimetric analyzer, aided with X-ray diffraction (XRD) analyses and SEM-EDS analyses, were used to investigate the effects of reaction atmospheres, temperatures, pressures and ash composition on the mineralogical transformation of coal ash during pressurized fluidized bed combustion and gasification. The results showed that the pressure had obvious influences on the transformation of mineral under different reaction atmosphere. The pressure facilitated the transformations of oldhamite into anhydrite and the fusion of hematite and suppressed the decomposition of the fluxing minerals like muscovite and anhydrite under the gasification atmosphere. The influence of pressure on the mineral types was not obvious but only facilitated the transformations of the muscovite and microcline into mullite and the albite under the inertia and combustion atmospheres. The effect of temperature on the ash fusion characteristics was strongly dependent on the atmospheres. In gasification atmospheres, the iron-bearing minerals and feldspar minerals, such as hercynite and anorthite, became abundant and reacted with other minerals to form low-temperature eutectics, thus decreasing the fusion temperatures. In combustion atmospheres, more high temperature minerals such as sanidine and mullite were formed and dominate, leading to increases in the fusion temperatures. With the increase in Fe2O3, there were muscovite, magnetite and anhydrite, etc. in the combustion atmosphere, resulting in the decrease of the fusion temperature. In the gasification atmosphere, hercynite and albite were detected, which can react with other minerals to form low temperature eutectics. With increasing the CaO, there were the fluxing minerals (anhydrite, and hematite) and some feldspar minerals, such as calcite and gehlenite, easy to produce low-temperature eutectics with other minerals, and hereby declining the fusion temperature in the combustion atmosperes. In the gasification atmosphere, the anorthite was present along with anhydrite, hematite, calcite and gehlenite. With the increase in Na2O, there were fluxing minerals, such as muscovite, magnetite, anhydrite and nepheline in the combustion atmosphere; there were the fluxing minerals like nepheline and the minerals, like gehlenite, easy to produce low-temperature eutectics with other minerals, leading to the reduction of the fusion temperature.
(3) AFTs were examined under different atmospheres and ash composition using ash fusion determinator. The effects of chemical components of ash and reaction atmospheres on the ash fusion behaviors have been analyzed under typical gasification and combustion atmospheres, aided with the FactSage software. The results indicated that with increasing the Fe2O3,CaO and Na20contents under the combustion and gasification atmospheres, the four temperatures DT, ST, HT and FT declined dramatically. With the increase in Fe2O3, CaO and Na2O contents, the generation and transformation of minerals occurred. The iron-containing minerals, such as hercynite and fayalite, were formed as increased the content of Fe2O3; the Ca-bearing feldspar minerals, like anorthite and gehlenite, were present with increasing the CaO content; and the Na-containing feldspar minerals, like carnegiete etc., were detected as the Na2O was increased. These three minerals can form low temperature eutectics, decreasing the fusion temperature.
(4) Based on the experimental results, the mineral distributions under different temperatures and pressures were displayed using the phase theory. The mechanism of ash fusion was analyzed using the phase theory. The effect of temperature on the mineral transformations was significant while the effect of pressure was not obvious. Meanwhile the atmospheres which the minerals were in were related to the effects of temperature and pressure. The transformations of minerals under gasification atmosphere were more than under the combustion atmosphere.
This indicated that more phase transformations occurred under the gasification atmosphere than the combustion atmosphere. With increasing the temperature, the Fe2+-bearing minerals, like hercynite, reacted with SiO2, Al2O3in ash to form iron-containing minerals like hercynite and fayalite etc. under the reducing atmosphere. The feldspar minerals, such as anorthite and microcline, were formed by the reactions between the alkali and alkali earth oxides and the SiO2Al2O3in the oxidizing atmosphere. In general, the feldspar minerals and the iron-bearing minerals can react with other minerals, such as Na2O·2SiO2、K2O·4SiO2, to form low temperature eutectics like Na2O·2SiO2+SiO2+Na2O·3CaO·6SiO2. With the increase in pressure, the mineral transformations are not obvious in the oxidizing and inert atmospheres, however, the pressure affects the crystallization of minerals. Moreover, the fluxing minerals like muscovite and anhydrite coexisted and produced low temperature melting. Pressure facilitated the form of the feldspar minerals, like anorthite, sanidine etc. in the gasification atmosphere. The feldspar minerals can form the low temperature eutectics.
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