第59卷第11期化工學(xué)報(bào)vol2008年11月Journal of Chemical Industry and Engineering (China)November 2008研究論文水煤漿氣流床氣化過程中氮的遷移陳忠,袁帥,梁欽鋒,王輔臣,囝遵宏(華東理工大學(xué)煤氣化教育部重點(diǎn)實(shí)驗(yàn)室,上海200237)摘要:在四噴嘴對(duì)置式氣流床氣化爐中,考察了水煤漿在不同氧碳比氣化條件下HCN、NH3、NO和N2的軸徑向濃度。結(jié)果表明:氮污染物(HCN、NH3、NO)在噴嘴平面處即產(chǎn)生并濃度最高,其主要來源于煤?？焖贌峤鈺r(shí)析出的揮發(fā)分,遠(yuǎn)離噴嘴平面時(shí)三者濃度大幅降低并大多轉(zhuǎn)化為N2,且氧碳比增高有利于N2的生成,氣化室出口處濃度N2>HCN>NH1>NO;流場(chǎng)分布使氣化室出口附近徑向濃度基本一致,而其上部各平面位置靠近爐壁處濃度較低;煤漿中的適量水分有利于HCN和NH3生成,但過量水分不利于揮發(fā)氮析出,使HCNNH3和NO生成量降低關(guān)鍵詞:水煤漿;氣流床;氮;遷移中圖分類號(hào):TQ546文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):0438-1157(2008)11-2884-07Release of nitrogen during coal water slurrygasification in entrained-flow gasifierCHEN Zhong, YUAN Shuai, LIANG Qinfeng, WANG Fuchen, YU Zunhong(Key Laboratory of Coal Gasification of Ministry of Education, East China University ofScience and Technology, Shanghai 200237, ChinAbstract: Various axial and radial concentrations of HCN, NH3, NO and N2 were measured during thegasification of coal water slurry (CwS)in a laboratory opposed multi-burner gasifier. The results showedthat the majority of nitrogen pollutants(HCN, NH, and NO) came from the release of volatile nitrogen ofcoal during the rapid heating process of devolatilization. The maximum concentrations of nitrogenpollutants were produced at the nozzle plane and decreased away from the plane; moreover, the ordering inthe aft-region was N2 >HCN>NH3>NO Increase of O2/C ratio tended to favor the formation of N2Flowfield distribution led to uniform radial concentrations at the exit and low concentrations near the side-wallin other axial positions. a proper amount of water in CWS tended to favor the formation of HCN andNH,. However, the introduction of excessive steam played a role in restraining the release of volatilenitrogen and reducing the concentrations of HCN, NH; and NOKey words: coal water slurry; entrained-flow gasifier; nitrogen; release引言轉(zhuǎn)化率高、粗煤氣質(zhì)量好等特點(diǎn)成為目前應(yīng)用范圍最廣、工藝最成熟的氣流床氣化技術(shù)。工業(yè)生產(chǎn)表水煤漿氣化以其原料范圍寬、安全易控制、碳明,氣化時(shí)煤中的氮(N)會(huì)轉(zhuǎn)化為HCN、NH3、2008-03-31收到初稿,2008-07-01收到修改稿中國(guó)煤化工聯(lián)系人;王輔臣。第一作者:陳忠(1980—),男,博士研究dYHCNMHG金項(xiàng)目:長(zhǎng)江學(xué)者和創(chuàng)新團(tuán)隊(duì)發(fā)展計(jì)劃項(xiàng)目(IT0620);教育部新世紀(jì)人才支持計(jì)劃”項(xiàng)目(NCET050415第11期陳忠等:水煤漿氣流床氣化過程中氮的遷移·2885N2和少量NO。粗煤氣在洗滌、凈化過程中一部camera poarch crown分NH3和HCN仍然會(huì)存在于合成氣中;另一部分則聚集在工藝系統(tǒng)的洗滌冷凝水中。產(chǎn)生的NH3和HCN,在煤氣化聯(lián)合循環(huán)發(fā)電(IGCC)nozzles中,將是NO2的前驅(qū)物;在甲醇洗工段NH3會(huì)降castabl低脫硫效果,導(dǎo)致尿素工段脫氫鉑催化劑中毒;系nsulation統(tǒng)水中過量NH的存在會(huì)使系統(tǒng)水pH值偏高,gasifier ex影響穩(wěn)定劑效果,并使溶解的碳銨( NH HCO3)sample port和CaCO3在系統(tǒng)低溫處析出,磨蝕、堵塞設(shè)備和管路,系統(tǒng)壓力升高;廢水中也因含NH3和HCN圖1氣化爐結(jié)構(gòu)示意圖而污染環(huán)境。目前,生產(chǎn)中需排放大量冷凝液并向Fig 1 Schematic diagram of gasification reactor系統(tǒng)中補(bǔ)充新鮮水以緩解問題,但是補(bǔ)水量大、資源耗用多,冷凝液再生、循環(huán)動(dòng)力能耗高,處理效擊。實(shí)驗(yàn)中先用柴油點(diǎn)火并烘爐4h左右,再切換果和經(jīng)濟(jì)性并不令人滿意,。因此,從氣化反應(yīng)機(jī)理為水煤漿進(jìn)料上對(duì)煤中氮的轉(zhuǎn)化規(guī)律進(jìn)行研究,以期達(dá)到源頭污實(shí)驗(yàn)在如下兩個(gè)條件下進(jìn)行,條件a:氧碳比染控制,對(duì)于發(fā)展低污染、低能耗的煤基發(fā)電和化(m23:kg1)0.6、0.8、1.0、1.2和1.4,純氧學(xué)工業(yè)具有重要意義,并已成為國(guó)內(nèi)外研究者和工(99.6%)氣化;條件b:在條件a下頂部附加流程技術(shù)人員的共識(shí)。量1.1ml·s-1的水氣。分別考察了氣化爐軸向6目前,煤中N的熱解、氣化研究多集中在較個(gè)位置及相應(yīng)徑向5個(gè)位置HCN、NH3、NO和小的固定床、流化床反應(yīng)器中1,而針對(duì)大型工N2的濃度,實(shí)驗(yàn)流程見圖2。徑向位置選取距中業(yè)氣流床氣化爐型的研究很少;實(shí)驗(yàn)條件與工業(yè)實(shí)軸線0、4、8、11和15cm處,軸向位置以噴嘴平際也存在較大差距,如氣化溫度不夠高、進(jìn)料量不面(3“)為基準(zhǔn)記為0cm,噴嘴平面上部取樣位夠強(qiáng),氣化介質(zhì)(原煤或煤粉)和氣化劑與工業(yè)實(shí)置(1、9和下部取樣位置(4"、5°、6”)分際不完全相符,水煤漿中的氮在氣流床氣化爐中的別記為負(fù)值和正值,其對(duì)應(yīng)關(guān)系見表1。轉(zhuǎn)化還未有報(bào)道。研究表明:不同爐型和氣化條表1軸向取樣位置與噴嘴平面距離件,煤中N的轉(zhuǎn)化規(guī)律也不盡相同。本研究在四Table 1 Distance between sample position噴嘴對(duì)置式氣流床氣化爐熱模實(shí)驗(yàn)平臺(tái)上,以工業(yè)用水煤漿和純氧為氣化介質(zhì)和氣化劑,考察了不同Axial position/ cm工藝條件下氣化爐中HCN、NH3、NO和N2的濃度分布。實(shí)驗(yàn)進(jìn)料量強(qiáng)、氣化溫度高,氣化爐型、氣化介質(zhì)和氣化劑與工業(yè)實(shí)際基本一致。1實(shí)驗(yàn)部分1.1實(shí)驗(yàn)裝置及實(shí)驗(yàn)方法1.2燃料特性實(shí)驗(yàn)用四噴嘴對(duì)置式氣化爐如圖1所示,由拱實(shí)驗(yàn)選用山東八一煤漿廠生產(chǎn)的水煤漿,其性頂、氣化室和急冷室組成,內(nèi)襯為剛玉管,內(nèi)徑質(zhì)見表2。30cm、高220cm,外部為不銹鋼外殼,中間隔有1.3檢測(cè)方法硅酸鋁保溫棉。沿氣化爐壁面開有熱電偶口和取樣實(shí)驗(yàn)中帶冷卻水冷凝的6根取樣管分別水平插孔,爐頂部有攝像儀口。同軸兩通道的4個(gè)噴嘴水入氣化室軸向6個(gè)預(yù)留取樣孔,以噴嘴平面處取樣平放置,兩兩對(duì)置,位于氣化爐上部同一平面。實(shí)為例中國(guó)煤化工接相應(yīng)的分析儀驗(yàn)中,水煤漿和氧氣由煤漿泵和質(zhì)量流量計(jì)分別以器CNMHG,檢測(cè)管中填塞恒定流量經(jīng)噴嘴內(nèi)、外通道高速噴入爐內(nèi),瞬間霧的特定鹵體切質(zhì)與傲極測(cè)氣及厘,使檢測(cè)管的化發(fā)生反應(yīng),并與對(duì)置噴嘴噴出的混合燃料氣撞段長(zhǎng)度變色至某一刻度從而讀取體積濃度。各物質(zhì)·2886·化工學(xué)報(bào)第59卷2水煤漿性質(zhì)Table 2 Properties of coal water slurryConcentration ViscosityProximate analysis/%(mass)Ultimate analysis/%(mass)Qber, v,oAsh fusion/%/mP, s Mo Aar Var FCr Cu Har Nr S o/M·kg1poin/℃67.2121532.86.90220738.2349.682840.950.436.419.30① As received basis;② By difference表3各物質(zhì)分析方法匯總Table 3 Summary of analysis methodsComponent Phase Analysis methoddetection limitsHCNHCN tube<±5%gas gas chromatography 2500 mvCO, H:, CO,, gas mass spectrometer 1 Hl.LCHe, Ar衰4不同氧碳比對(duì)應(yīng)的噴嘴平面溫度able 4 Relationship of O,/C and temperature圖2實(shí)驗(yàn)流程圖(O2/C)/m3kg-1Nozzle plane temperaFig 2 Flow sheet of experiment1--nozzle: 2-gasification furnace: 3-synthetic gas vent13614-cleaning and cooling room: 5-slag chamber14696--mass flowmeter: 7-electronic balance8-fuel storage tank: 9-gear pump: 10-vidiconaor mass spectrometer: 13--computer物(HCN、NH3和NO)均在噴嘴平面處濃度最高,遠(yuǎn)離噴嘴平面,三者濃度都大幅下降。說明nozzleCN、NH3和NO在霧化和撞擊時(shí)即可同時(shí)迅速生成,之后會(huì)轉(zhuǎn)化為其他含氮物而濃度降低。水煤nozzle漿氣化反應(yīng)是一個(gè)復(fù)雜的物理化學(xué)反應(yīng)過程,水煤漿和氧氣噴入氣化爐后瞬間經(jīng)歷煤漿升溫及水分蒸發(fā)、煤熱解揮發(fā)、殘?zhí)?char)氣化和氣體間的化學(xué)反應(yīng)等過程。煤中的氮大多以含氮雜環(huán)的形式存圖3噴嘴平面處取樣示意圖在,揮發(fā)分析出的是較重的烴類和芳香族化合ig. 3 Schematic plan of sampling物,煤顆粒中大部分氮(揮發(fā)氮)在這一步中以含method at nozzle plane氮芳環(huán)的形式釋放)。由于氧具有活化含氮雜環(huán)的分析方法見表3作用,再加之噴嘴平面高達(dá)1700℃的溫度,這些2結(jié)果與討論含氮雜環(huán)會(huì)很容易斷裂,進(jìn)而生成HCN、NH3和NO。21不同氧碳比時(shí)軸向各位置氮化物濃度由圖4~圖6可見,在氧碳比1.0時(shí)HCN和不同氧碳比對(duì)應(yīng)的氣化溫度見表4。NHV凵中國(guó)煤化工碳比時(shí)(14和圖4~圖7中分別為不同氧碳比條件下HCr0.CNMHG比0.6時(shí)最低,NH43、NO和N2的軸向位置濃度,其值為相應(yīng)徑隨氧碳比增高而增加,至1.4時(shí)濃度最高。煤中揮向數(shù)據(jù)的平均值?？梢?各氧碳比條件下,氮污染發(fā)氮( volatile-N)的析出速率取決于煤顆粒的受第11期陳忠等:水煤漿氣流床氣化過程中氮的遷移2887·O/C=1488z024axial location/cmaxial location/cm圖7軸向各位置N2濃度的變化圖4軸向各位置HCN濃度的變化Fig 7 Change of N, axial concentrationFig 4 Change of HCN axial concentrationNO的還原,部分HCN和NH3也會(huì)被氧化。圖6中出口處(6°,144cm)仍有較多NO,是由于實(shí)A驗(yàn)用氣化爐與工業(yè)爐相比,停留時(shí)間較短,轉(zhuǎn)化率1000不夠完全,出口處仍有一定氧化性氣氛所致,工業(yè)出口氣中NO應(yīng)很少。由圖4和圖5還可以看出,相同氧碳比時(shí)同一軸向位置NH3濃度比HCN低約100~200L-。這可能是因?yàn)樵跓峤膺^程中NH3的生成比HCN的生成緩慢10;另外,高溫下NH3更易分axial location/cm解也是出口處NH3較HCN低的原因之-(1從圖7可以看出,在噴嘴平面附近,N2濃度圖5軸向各位置NH3濃度的變化先減小,這說明氣化反應(yīng)中,火焰溫度超過Fig 5 Change of NH, axial concentration1500℃時(shí)純氧(99.6%)中0.4%的N2也會(huì)像燃燒反應(yīng)那樣與O2發(fā)生反應(yīng)生成NO°;隨著反應(yīng)進(jìn)行,遠(yuǎn)離噴嘴時(shí),在HCN、NH3和NO減少的同時(shí)N2濃度又增高,說明HCN、NH3和NO間相互轉(zhuǎn)化生成較多N2。隨著氧碳比升高,相同軸向位置處N2濃度增高,說明氧化性氣氛的增強(qiáng)有利于N2的生成。對(duì)比圖4~圖7發(fā)現(xiàn),在NH3、HCN和NO濃度降低的同時(shí)N2濃度雖然升高但三者中總N的減少量略小于N2中N的增加量10ial location/cm說明增加的N2并非完全來自最初生成的HCN、圖6軸向各位置NO濃度的變化NH3和NO,還有來自殘?zhí)恐袣埖? char-N)緩慢Fig 6 Change of NO axial concentration釋放出的含氮物熱情況,溫度升高,其析出速率增加。氧碳比2.2徑向位置氮污染物濃度0.6時(shí),氧氣量大幅減少,霧化效果變差、氣化溫氧碳比1.0時(shí)氮污染物徑向濃度如圖8~圖度降低,煤顆粒受熱速率減小,煤粒中揮發(fā)氮析出10,噴嘴平面處HCN、NH:和NO濃度最高,遠(yuǎn)速率和釋放量大幅降低,氧碳比增高氧濃度增加,離噴TⅥ中國(guó)煤化工至氣化室出口位氣化溫度顯著升高,煤粒揮發(fā)分析出速率和程度增置(CNMHG HCN、NH和高,但氧碳比過高會(huì)使較高比例的揮發(fā)氮直接被氧NO中心線廈相刈牧闕,幕近爐壁處較低?；蒒O。另外,氧化性氣氛的增強(qiáng)不利于后繼在噴嘴平面中心位置(0cm)HCN、NH3和NO·2888·化學(xué)第59卷濃度最高,靠近壁面處(15cm)濃度降低;在噴2.3流場(chǎng)對(duì)濃度分布的影響嘴平面上下2*、4“處,中心線(0cm)附近三者煤粒中氮的轉(zhuǎn)化過程與流場(chǎng)結(jié)構(gòu)密切相關(guān),可濃度較高,距中心線8cm時(shí)濃度大幅減少;在拱大致分為一次反應(yīng)和二次反應(yīng)。一次反應(yīng)是揮發(fā)分頂1·處,三者僅在距中心線11cm和15cm靠近中的揮發(fā)氮析出的同時(shí)含氮雜環(huán)裂解生成大量壁面處濃度降低較多;氣化室出口5“和6“處,徑HCN、NH3和NO,大部分燃料氮轉(zhuǎn)化為氣相含向濃度趨于一致。在其他氧碳比條件下也有類似氮物的過程,如式(1)所示,一次反應(yīng)的程度直規(guī)律接決定了HCN、NH3和NO的初始量。二次反應(yīng)包括:生成的HCN、NH3和NO間的相互反應(yīng);300三者與主要?dú)庀嘟M分(如CO、H2、CH4、CO2、1100H2O)和殘?zhí)款w粒的反應(yīng);殘?zhí)恐袣埖? char-N)進(jìn)一步釋放的反應(yīng),如式(2)~式(4)所示。olatile-n→HCN,NH3,NOoal-N→700CrH,,H cOHCN, NH3(2)NH, HCN6810121416radial location/cmcharN→N2,HCN,NH38HCN徑向濃度分布爐內(nèi)某個(gè)區(qū)域可能發(fā)生的轉(zhuǎn)化反應(yīng)是以一次反Fig8 HCN radial concentration profiles應(yīng)為主還是二次反應(yīng)為主,與該區(qū)內(nèi)的流體流動(dòng)特征及與之相應(yīng)的混合過程有關(guān)。氣化爐4股射流噴出后撞擊,在爐內(nèi)形成一定結(jié)構(gòu)的復(fù)雜流場(chǎng)21次反應(yīng)區(qū)包括射流區(qū)(I)和撞擊區(qū)(Ⅱ),由于噴嘴平面附近溫度很高,氧含量充足,此區(qū)域內(nèi)煤的脫揮發(fā)分及揮發(fā)分的裂解過程非常迅速,因此HCN、NH3和NO在噴嘴平面即可形成并濃度最高一次反應(yīng)區(qū)的產(chǎn)物HCN、NH3和NO在撞擊0246810121416擴(kuò)展區(qū)發(fā)生類似式(2)和式(3)的二次反應(yīng),隨radial location/cm著遠(yuǎn)離噴嘴平面而濃度降低,并大多生成了N2,圖9NH3徑向濃度分布形成了圖4~圖7所示的軸向濃度分布。殘?zhí)恐械腇ig 9 NH, radial concentration profiles殘氮也進(jìn)一步釋放,如式(4)所示,這一過程相對(duì)于式(2)和式(3)中的均相反應(yīng)過程是緩慢和次要的10由于射流的卷吸作用和湍流擴(kuò)散,在氣化爐壁面至射流(Ⅰ)和撞擊流股(Ⅲ)邊界形成了范圍較大的回流區(qū),在拱頂(1#)近爐壁處形成折返流區(qū)(V),這兩個(gè)區(qū)域內(nèi)進(jìn)行的也是二次反應(yīng)由于物料卷吸湍流程度大,各組分間接觸充分、停留時(shí)間長(zhǎng),二次反應(yīng)進(jìn)行更完全,從而使HCN、NH凵中國(guó)煤化工,形成了圖8~圖10CNMHG口(6),軸向速圖10NO徑向濃度分布度沿徑向分布基本保持不變,形成流場(chǎng)均勻的管流Fig. 10 No radial concentration profiles區(qū)(Ⅵ),區(qū)內(nèi)進(jìn)行的也是二次反應(yīng),但徑向濃度第11期陳忠等:水煤漿氣流床氣化過程中氮的遷移2889·差別不大2.4H2O對(duì)氮污染物生成量的影響3結(jié)論氣化時(shí)水煤漿中的水分可以為生成HCN和(1)水煤漿在四噴嘴對(duì)置式氣化爐中氣化時(shí)NH3提供必需的H自由基,NO也可被H自由基HCN、NH3和NO在噴嘴平面處即同時(shí)產(chǎn)生并于還原,從而使HCN和NH2的生成量較高,圖此處濃度最高,HCN和NH2不完全來自NO的后l1是氧碳比1.0時(shí)在氣化爐頂部附加流量為1.1繼還原,而主要是由煤?？焖贌峤馕龀龅膿]發(fā)分中nl·s-l水氣的實(shí)驗(yàn)結(jié)果。可以看出,HCN、NH3的含氮芳環(huán)裂解產(chǎn)生和NO濃度都有較多降低。這可能是由于煤漿中已2)各氧碳比下,初始濃度HCN>NH3>含有37.5%的水分,附加水氣后使水氣煤比由06NO,煤中的氮轉(zhuǎn)化為HCN較生成NH和NO容升高為0.73,過高的水氣煤比可使峰值溫度和煤易、直接;NO濃度隨氧碳比增加始終增高;而粒加熱速率降低,從而導(dǎo)致?lián)]發(fā)氮析出減少,同HCN和NH在氧碳比1.0時(shí)最高,增高和降低氧時(shí),氣體中高水氣的存在還使氧濃度降低,不利于碳比二者濃度降低。揮發(fā)氮裂解,并改變氧與揮發(fā)氮的氣相反應(yīng)速率,(3)隨氣化反應(yīng)進(jìn)行,HCN、NH3和NO濃HCN、NH3和NO生成量降低:1。度降低,并較多轉(zhuǎn)化為N2,氣化室出口處N2濃度最高;氧碳比增高有利于N2的生成(4)含氮物的濃度分布與爐內(nèi)流場(chǎng)的分布密切相關(guān)。(5)煤漿中的一定量水分有利于HCN和NH的生成,但過高水氣煤比時(shí)氮污染物生成量降低,原因是氣化效果變差,揮發(fā)氮析出和裂解受到影響。200References140axial location/cm[1 Takeharu Hasegawa, Mikio Sato. 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