第40卷第1l期燃料化學(xué)學(xué)報(bào)Vol 40 No 112012年11月Journal of Fuel Chemistry and TechnologyNov,2012文章編號(hào):0253-2409(2012)11-128906腐植酸型煤氣化特性及動(dòng)力學(xué)研究崔國星,林明穗(三明學(xué)院化學(xué)與生物工程學(xué)院,福建三明365004摘要:以低活性福建無煙粉煤為原料,采用腐植酸型煤黏結(jié)劑,制得腐植酸型煤。比較研究型煤和無煙煤在常壓條件下的氣化動(dòng)力學(xué)和氣化特性。運(yùn)用等溫?zé)嶂胤?在900~1150℃進(jìn)行水蒸氣氣化實(shí)驗(yàn),測定了型煤和無煙煤的反應(yīng)速率、轉(zhuǎn)化率與時(shí)間的關(guān)系,考察了常壓下溫度和煤樣對(duì)氣化反應(yīng)的影響。釆用積分縮核模型對(duì)實(shí)驗(yàn)數(shù)據(jù)進(jìn)行擬合關(guān)聯(lián),得到煤樣水蒸氣氣化反應(yīng)的動(dòng)力學(xué)參數(shù)。結(jié)果表明,型煤的氣化反應(yīng)活化能(102.0kJ/mol)低于福建無煙煤(12.5kJ/mo)。950℃下型煤的化學(xué)反應(yīng)性(80.0%)優(yōu)于福建無煙煤(33.0%)。型煤較福建無煙煤表現(xiàn)岀更好的化學(xué)反應(yīng)性,可代梼優(yōu)質(zhì)塊煤用于工業(yè)固定床煤氣化。關(guān)鍵詞:型煤;氣化動(dòng)力學(xué);等溫?zé)嶂胤?氣化特性;化學(xué)反應(yīng)性中圖分類號(hào):TQ541文獻(xiàn)標(biāo)識(shí)碼:AGasification characteristics and kinetics of briquette using humic acid binderCUI Guo-xing, LiN Ming-suiSchool of Chemical and Biological Engineering, Sanming University, Sanming 365004, China)Abstract: Briquette was made from a low active pulverized Fujian anthracite with humic acid as binder. Thegasification reaction kinetics and characteristics of briquette were compared with those of Fujian anthracite, Thesteam gasification rate was determined at the temperature of 900-1 150 C and atmospheric pressure by using theisothermal thermogravimetry. The kinetic parameters of gasification were calculated based on the shrinking-coremodel SCM). The data show that the activation energy of briquette is 102.0 kJ/mol, lower than that of Fujiananthracite(122.5 kJ/mol). The carboxyreactivity of briquette is 80. 0% at 950 C, while it is only 33. 0% forujian anthracite granule. The results exhibit that the briquette has a higher gasification reactivity than FujianFanthracite lump, and could be a substitute of high quality lump coal for the industrial fixed bed gasificationKey words: briquette; gasification kinetics; isothermal thermogravimetry; gasification characteristicscarboxyreactivity屮國少油富煤,煤炭資源豐富。絕大部分氮肥、化動(dòng)力學(xué)規(guī)律。目前,對(duì)型煤的化學(xué)反應(yīng)性研究較甲醇等化工企業(yè)均以優(yōu)質(zhì)無煙塊煤為原料,氣化生少,型煤氣化動(dòng)力學(xué)的研究文獻(xiàn)報(bào)道較少產(chǎn)合成氣氫氣和工業(yè)及民用燃?xì)狻５捎诿簩颖狙芯窟\(yùn)用等溫?zé)嶂胤?以水蒸氣為氣化劑,考中自然塊煤率及爆破開采、機(jī)械化采煤時(shí)部分塊煤察煤種和反應(yīng)溫度對(duì)氣化過程的影響,及常壓條件粉碎的原因,造成無煙塊煤供應(yīng)不足而粉煤積壓。下水蒸氣的氣化速率。開展型煤氣化反應(yīng)動(dòng)力學(xué)和低價(jià)值粉煤成型可拓寬氣化原料來源,提高煤資源氣化特性的研究,將為氣化條件優(yōu)化、反應(yīng)器選型和利用率,并在固定床氣化爐上進(jìn)行工業(yè)化成用2工程放大設(shè)計(jì)等提供理論基礎(chǔ),對(duì)推動(dòng)工業(yè)型煤潔實(shí)現(xiàn)了節(jié)能減排的目標(biāo)。隨著膜法富氧技術(shù)等新型凈氣化具有現(xiàn)實(shí)意義。富氧制備工藝技術(shù)的發(fā)展,型煤燃燒富氧氣化具有1實(shí)驗(yàn)部分良好的工業(yè)發(fā)展前景。1.1實(shí)驗(yàn)原料型煤氣化反應(yīng)性和動(dòng)力學(xué)特性對(duì)揭示型煤氣化從三明化工有限公司工業(yè)氣化用腐植酸型煤中規(guī)律、提高氣化效率、實(shí)現(xiàn)煤高效轉(zhuǎn)化極其重要。世采樣,該型煤的制作方法為,以3m以下低活性的界各國研究者釆用常壓或加壓熱重法研究了福建無煙粉煤及少量下腳料(回料,為無煙粉煤,含煤焦與水蒸氣或CO28反應(yīng)活性和氣化動(dòng)力學(xué)碳較低),摻加少量煙煤粉為原料,添加腐植酸型煤林榮英等探討了低活性無煙煤二氧化碳催化氣黏結(jié)劑拌勻、漚化,用壓輥冷壓成型為扁平橢球狀濕收稿日期:201202-15;修回日期:201240430基金項(xiàng)目:福建省科技計(jì)劃重大項(xiàng)目(2010H6020);福建省科技計(jì)劃項(xiàng)目(2010H2006)。聯(lián)系作者:崔國星(1961-),男,福建莆田人,碩土,副教授,主要從事能源化工工藝教學(xué)與研究。Emt:fimg@163.com1290燃料化學(xué)學(xué)報(bào)第40卷球,在隧道窯中經(jīng)過600℃扃溫?zé)煹罋夂娓芍频酶?briquette)和福建大田無煙煤( Fujian anthracite)的組植酸型煤。實(shí)驗(yàn)選用的腐植酸型煤( Humic acid成性質(zhì)見表1。表1腐植酸型煤和福建大田無煙煤的性質(zhì)分析Table 1 Properties analysis of Humic acid briquette and Fujian anthraciteProximate analysis w ad/%oUltimate analysis w ad/%Net calorific valuesamMFCHQ/(M·kgHumic acid briquette2.2266.626.0225.1467.171.312.880.680.60Fujian anthracite4.3573.693.2218.7472.740.662.540.520.4524.8812實(shí)驗(yàn)儀器和方法學(xué)反應(yīng)性的指標(biāo)。儀器:STA449P3同步熱分析儀(配水蒸氣爐)3氣化數(shù)據(jù)分析(天平分辨率:0.1μg),德國 NETZSCH公司,用于由同步熱分析儀計(jì)算機(jī)自動(dòng)采樣繪出失重曲線煤樣氣化時(shí)質(zhì)量損失的測量;水蒸氣發(fā)生器及傳輸(TG曲線),得到重量溫度時(shí)間的相關(guān)原始數(shù)據(jù),系統(tǒng), Bronkhorst高技術(shù)有限公司,用于產(chǎn)生定量的利用(1)式計(jì)算煤樣-水蒸氣氣化碳轉(zhuǎn)化率x,%,繪水蒸氣供煤氣化;HX1煤炭活性測定儀,杰韋弗出轉(zhuǎn)化率和時(shí)間t關(guān)系圖(x~t)。(中國)公司,用于煤樣的化學(xué)反應(yīng)性測定。100%熱重實(shí)驗(yàn):將型煤和福建無煙煤樣粉碎磨細(xì)到l0(1-M-V-A')0.15mm(100目)以下細(xì)粉供熱重實(shí)驗(yàn)。每次稱取50mg煤樣,置于同步熱分析儀剛玉(Al2O3)坩堝dx-測y+w(I-M-V-A)100%中。實(shí)驗(yàn)前將同步熱分析儀接通電源,打開循環(huán)冷式中,w0為初始煤樣的質(zhì)量,mg;to、m,分別卻水,以高純氮?dú)鉃楸Ｗo(hù)氣和吹出氣(流量均為為開始通水蒸氣氣化(L=0)和任意時(shí)刻t時(shí)煤樣的20mL/min),分別置換保護(hù)天平室及吹出氣化爐質(zhì)量,mg;V、A'、M分別為煤樣中揮發(fā)分灰分、中的空氣或反應(yīng)氣,保證實(shí)驗(yàn)環(huán)境,儀器預(yù)熱穩(wěn)定水分的質(zhì)量分?jǐn)?shù)。3h后開始測試。放入煤樣后,按設(shè)定的升溫速率曲用同步熱分析儀 Proteus分析軟件,對(duì)失重曲線線加熱至所需氣化溫度。從常溫至反應(yīng)溫度前作一階微分,即DG曲線,得-d,/dt,失重速率。50℃升溫速率為20℃/min,恒溫5min后,以利用式(2)計(jì)算得氣化反應(yīng)速率dx/d,繪得反應(yīng)3℃/min速率升溫到指定氣化溫度。達(dá)到設(shè)定反應(yīng)速率對(duì)時(shí)間關(guān)系曲線(xd-t)溫度后,接入水蒸氣進(jìn)行氣化反應(yīng),并維持恒溫。2結(jié)果與討論水燕氣流量6g/h(124mL( NPT)/min),每次2.1熱重實(shí)驗(yàn)分析實(shí)驗(yàn)前進(jìn)行流量校正,經(jīng)過加熱裝置后完全氣化,與2.1.1溫度對(duì)型煤氣化反應(yīng)的影響高純N2吹出氣一起穩(wěn)定送入氣化反應(yīng)爐,水蒸氣在整個(gè)煤氣化反應(yīng)過程,樣品量少,故反應(yīng)量也180℃,傳輸管道150℃保溫,水蒸氣分壓為少,水蒸氣過量,則生成一氧化碳和氫氣所占的比例0086MPa實(shí)驗(yàn)完畢,繼續(xù)通氮冷卻至200℃后,將很小,水蒸氣加入量和高純N2吹出氣保持不變,水坩堝取出,觀察煤樣形態(tài)。蒸氣的分壓(0.086MPa)視為恒定。型煤細(xì)粉和?；瘜W(xué)反應(yīng)性測定:按照GB/T220-2001《煤的建無煙煤細(xì)粉在不同溫度下氣化反應(yīng)速率與氣化時(shí)化學(xué)反應(yīng)性測定方法》,先將型煤球和無煙煤塊破間的關(guān)系見圖1。碎后,以17.5℃/mn的速率升溫到900℃干餾1h由圖1可以看出,型煤和福建無煙煤的氣化反除去揮發(fā)分。冷卻后篩分選取3~6mm粒徑的焦應(yīng)速率均呈山峰狀變化。溫度越高,速率曲線的山渣粒裝入煤炭活性測定儀的反應(yīng)管(管內(nèi)徑φ峰越明顯,其最大反應(yīng)速率隨之明顯增大,反應(yīng)越激22mm,料層高H100mm)中加熱到一定溫度后,以烈。煤樣與水蒸氣反應(yīng)時(shí)間為3.0~4.0min時(shí),反規(guī)定的流量通入二氧化碳與試樣反應(yīng)。測定反應(yīng)后應(yīng)速率達(dá)最大;隨著反應(yīng)溫度升高,達(dá)到最大氣化反氣體中二氧化碳的含量,以被還原成一氧化碳的ˉ.應(yīng)速率峰值所需的時(shí)間略有縮短,而最終完成反應(yīng)氧化碳量占通入的二氧化碳量的百分?jǐn)?shù),即二氧化的時(shí)間明顯減少。超過一定反應(yīng)時(shí)間后,高溫下的碳還原率α(%),作為型煤和無煙煤對(duì)二氧化碳化氣化反應(yīng)速率反而較低溫下低,各溫度所對(duì)應(yīng)的氣第11期崔國星等:腐植酸型煤氣化特性及動(dòng)力學(xué)研究1291化速率出現(xiàn)交叉的位置隨著反應(yīng)溫度升高的時(shí)間提緣故。前(。這是由于此時(shí)高溫下碳轉(zhuǎn)化率高,剩碳少的12(a)60102060Reaction time 4/minReaction time t/min圖1型煤和福建無煙煤在不同溫度下氣化反應(yīng)速率與氣化時(shí)間的關(guān)系Figure 1 Relationship between gasification rate and reaction time of powder sample at different temperature(a): Humic acid briquette;(b): Fujian anthacite口:1150℃;o:1100℃;Δ:1050℃;V:100℃;◇:950℃;<:900℃2.12型煤和無煙煤氣化反應(yīng)速率的比較2.2氣化動(dòng)力學(xué)參數(shù)的計(jì)算型煤細(xì)粉和福建無煙煤細(xì)粉具有相近粒徑分2.2.Ⅰ氣化動(dòng)力學(xué)參數(shù)的微分模擬布,在相同氣化劑流量條件下發(fā)生氣化反應(yīng)。不同煤樣氣化混合反應(yīng)模型氣化速率微分式:煤樣碳-水蒸氣氣化在同一碳轉(zhuǎn)化率(x=25%)時(shí)(3)氣化反應(yīng)速率與溫度的關(guān)系,見圖2。由圖2可看dt- roexp (-E/RT)(1-x)出,在相同氣化反應(yīng)溫度下,經(jīng)過同一碳轉(zhuǎn)化率反應(yīng)式中,指數(shù)m具有經(jīng)驗(yàn)意義,不同煤種具有不后,型煤和福建無煙煤的氣化反應(yīng)速率基本相近,差同m值。即(1-x)的指數(shù)可能是1或2/3之間異較小。型煤以福建無煙粉煤為原料煤,摻加少量的某個(gè)值,m等于1時(shí)為均相反應(yīng)模型,2/3時(shí)符合煙煤粉,添加腐植酸型煤黏結(jié)劑制成,熱重實(shí)驗(yàn)時(shí),縮核反應(yīng)模型。在升溫加熱至氣化反應(yīng)溫度過程,煙煤和腐植酸型根據(jù)dκ/dt~t和x~t關(guān)系,得出型煤細(xì)粉煤黏結(jié)劑所含揮發(fā)分基本揮發(fā)殆盡,型煤和福建無dwdt~x關(guān)系,見圖3煙煤煤樣在升溫加熱過程干餾變焦,在基本消除擴(kuò)2散的條件下氣化,反應(yīng)速率取決于焦的氣化反應(yīng)活c一日一u一口性,兩者差異不大,因而反應(yīng)速率基本相近。0→-0-Fujian anthracite6E10o-Humic acid briquett8Conve圖3型煤水燕氣氣化反應(yīng)速率與碳轉(zhuǎn)化率的關(guān)系0L1,1Figure 3 Relationship between gasification rate and9501000105011001150conversion of briquette powderGasification temperature //CLegends: see Figure 1圖2不同溫度下型煤和福建無煙煤在x=25%時(shí)的氣化速率通過 MATLAB軟件對(duì)式(3)進(jìn)行多元非線性回Figure 2 Gasification rate of powder sample歸,直接計(jì)算出型煤的混合反應(yīng)模型氣化動(dòng)力學(xué)指in 25 carbon conversion at different temperature數(shù)m和氣化反應(yīng)活化能E及頻率因子k。從回歸1292燃料化學(xué)學(xué)報(bào)第40卷結(jié)果看,混合反應(yīng)模型氣化動(dòng)力學(xué)指數(shù)m和氣化反222氣化動(dòng)力學(xué)參數(shù)的積分關(guān)聯(lián)應(yīng)活化能E及頻率因子k,皆在合理值范圍。但叫采用未反應(yīng)縮核模型( shrinking core model歸殘差呈一定的規(guī)律性,在x較低和較高時(shí)為負(fù)偏SCM)計(jì)算煤氣化動(dòng)力學(xué)參數(shù)),其數(shù)學(xué)表達(dá)式簡差,在中間值時(shí)x呈正偏差,這表明實(shí)測數(shù)據(jù)與模型單,并具有足夠精度。的吻合程度不好。從圖4模擬式(3)的型煤細(xì)粉氣未反應(yīng)縮核模型:化dx/d~x關(guān)系曲線,與圖3實(shí)測值的比較,可看dx/dt=k(1-x)23出兩者差異。一些研究者也指出等溫?zé)嶂胤ù嬖谖捶磻?yīng)縮核模型積分式6零時(shí)間”影響12。運(yùn)用等溫?zé)嶂胤?得到dx/dt~x3[1-(1-x)1/3I=h t(5)關(guān)系,以微分法通過多元非線性回歸計(jì)算混合反應(yīng)型煤細(xì)粉和福建無煙煤細(xì)粉在不同反應(yīng)溫度下模型氣化動(dòng)力學(xué)參數(shù)的方法不可行。碳轉(zhuǎn)化率與時(shí)間的關(guān)系,見圖5。根據(jù)x-t關(guān)系以3[1-(1-x)對(duì)反應(yīng)時(shí)間t作圖,得圖6,從k=045×10,E=955 kJ/mol.m=06667回歸得到斜率,即該煤樣在各氣化反應(yīng)溫度的速率常數(shù)k,結(jié)果見表2。根據(jù) Arrhenius經(jīng)驗(yàn)方程:k=hg exp(-E,RT)式中,E。為氣化反應(yīng)活化能,如溫度變化不大可看為常數(shù),k為頻率因子,R為氣體常數(shù)。將此經(jīng)驗(yàn)方程兩邊取對(duì)數(shù)得:Ink= lnko-E/RT010203040506070809010Conversion x%對(duì)每個(gè)煤樣,根據(jù)不同氣化反應(yīng)溫度下的k圖4模擬的型煤水蒸氣氣化速率與轉(zhuǎn)化率的關(guān)系T關(guān)系,以hnk對(duì)相應(yīng)溫度1/T作圖,見圖7,根conversion of briquette powder by mixed reaction moder BadFigure 4 Simulation relationship between gasification rate據(jù)回歸的斜率和截距可得到各煤樣的氣化反應(yīng)活化能E及頻率因子k,結(jié)果見表3。(a)403000Reaction time //minReaction time t/min圖5型煤和福建無煙煤在不同反應(yīng)溫度下碳轉(zhuǎn)化率與時(shí)間的關(guān)系Figure 5 Relationship between carbon conversion percent and reaction time of powder sample at different temperature(a): Humic acid briquette; (b): Fujian anthaciteLegends: see Figure 1表2型煤和福建無煙煤氣化速率常數(shù)kx102和相關(guān)系數(shù)p2Table 2 Gasification rate constant h x10 and correlation coefficient p of briquette and anthracite granuleT/KI173I27313231373142Humic acid briquette h x10/min7.519.471.9815.070.99890.99870.99730.997499670.9963Fujian anthracitek×1032/min-11.956.5014.317.55Powder0.99720.99910.99890.99780.99640.9956第11期崔國星等:腐植酸型煤氣化特性及動(dòng)力學(xué)研究1293回歸相關(guān)系數(shù)ρ?2主要反映了模型缺欠和實(shí)驗(yàn)略低于福建無煙煤細(xì)粉的12.5kJ/molb與以往水誤差等因素對(duì)模型回歸的影響程度,可檢驗(yàn)一個(gè)模蒸氣氣化反應(yīng)實(shí)驗(yàn)結(jié)果比,該反應(yīng)活化能與相關(guān)文型吻合度。從表2、表3可知,此模型具有很好的相獻(xiàn)基本吻合關(guān)性。從E值看,型煤細(xì)粉氣化活化能為1020kJ/mol,2.020.660.880.00Reaction time //minReaction time t/min圖6型煤和福建無煙煤的3[]-(1-x)1與氣化反應(yīng)時(shí)間的關(guān)系igure 6 Relationship between 3[1-(1-x)3] and gasification time of powder sample at different temperature(a). Humic acid briquette; (b): Fujian anthaciteLegends: see Figure 1表3型煤和福建無煙煤的氣化動(dòng)力學(xué)參數(shù)化。由于高溫時(shí)氣化速率較快,型煤和福建無煙煤1abe3 Gasification kinetics parameter of powder sample都使通入二氧化碳還原轉(zhuǎn)化接近完全,所以所測的Coal powder sample E/(kImol-)k,/min化學(xué)反應(yīng)性差異縮小。一般以950℃下的測量值來Humic acid briquette102.0941.10.9819衡量煤樣的化學(xué)反應(yīng)性。950℃下型煤的化學(xué)反應(yīng)Fujian anthracite12256384.60.9907性為80.0%,顯著高于福建無煙煤的30%,這和note: Ea: reaction activation energy; k,: pre-exponential factor型煤與無煙煤的結(jié)構(gòu)差異有關(guān)。2.3型煤和無煙煤化學(xué)反應(yīng)性的比較測定90-1100℃下型煤和福建無煙煤的化學(xué)反應(yīng)性,結(jié)果見圖8。880b60id briquette20fisting3.0204.0口- Humic acid briquetteFujian anthraxFujian anthracite95010001050Temperature [/C圖8不同溫度下型煤和福建無煙煤的化學(xué)反應(yīng)性能Figure 8 Carboxyreactivity of briquette and anthracite granule7072747.6788.0828486L*10+K型煤主要由無煙煤粉組成,兩者細(xì)粉化學(xué)反應(yīng)圖7型煤和福建無煙煤氣化反應(yīng)的 Arrhenius圖性和氣化速率差異不大,但型煤與福建無煙煤的理Figure 7 Arrhenius chart of powder sample gasification化性質(zhì)不同。型煤由3mm以下煤粉用黏結(jié)劑黏接,從圖8可看出,不同溫度下測得的化學(xué)反應(yīng)性高溫烘于而成,由于架橋形成疏松多孔結(jié)構(gòu),較致密不同。隨著二氧化碳?xì)饣磻?yīng)溫度升高,煤樣分子的福建無煙煤塊具有更大的比表面積。型煤制作越來越多地能夠越過能壘進(jìn)行反應(yīng)型煤和福建無時(shí),所加人的黏結(jié)劑腐植酸和少量煙煤,在高溫烘于煙煤的化學(xué)反應(yīng)性都得到提高,即高溫有利于煤氣過程中因揮發(fā)分的脫除,形成孔隙,使型煤的孔結(jié)構(gòu)1294燃料化學(xué)學(xué)報(bào)第40卷進(jìn)一步發(fā)達(dá),孔隙率高,比表面積大,氣化劑易與固采用微分法進(jìn)行多元非線性回歸,計(jì)算型煤氣體表面接觸3),化學(xué)反應(yīng)性得到提高?？梢?型化混合模型的氣化動(dòng)力學(xué)參數(shù),呈現(xiàn)規(guī)律性的回歸煤作為氣化原料具有較奷的反應(yīng)性,氣化反應(yīng)速率殘差,效果不好。用積分法氣化縮核模型關(guān)聯(lián)型煤快,利于煤轉(zhuǎn)化,可替代優(yōu)質(zhì)塊煤,用于T業(yè)固定床氣化實(shí)驗(yàn)數(shù)據(jù),簡便可行,得岀型煤水蒸氣氣化動(dòng)力煤氣化。學(xué)參數(shù)精度高,與文獻(xiàn)吻合。說明應(yīng)用等溫?zé)嶂胤?3結(jié)論對(duì)型煤進(jìn)行氣化動(dòng)力學(xué)實(shí)驗(yàn)研究的方法是可行的。恒溫下水蒸氣氣化溫度越高,腐植酸型煤的反型煤氣化活化能為102.0kJ/mol,低于福建無應(yīng)速率越快,相同時(shí)間下相應(yīng)轉(zhuǎn)化率越大,完成反應(yīng)煙煤的122.5kJ/mol950℃下型煤的化學(xué)反應(yīng)性所需時(shí)間縮短。型煤的反應(yīng)速率呈單峰趨勢,且在(80.0%)優(yōu)于福建無煙煤(330%)。低活性的福反應(yīng)進(jìn)行3.0~4.0min時(shí)達(dá)到最大值,然后反應(yīng)速建無煙粉煤摻加少量煙煤粉,采用腐植酸型煤黏結(jié)率降低。隨反應(yīng)溫度升高,煤樣反應(yīng)達(dá)到最大反應(yīng)劑,制得的型煤作為氣化原料具有較高的反應(yīng)性,可速率所需的時(shí)間略有縮短。代替塊煤,用于工業(yè)固定床氣化。參考文獻(xiàn)1]崔圖星,王文生,張啟衛(wèi).型煤移動(dòng)末富氧連綏氣化系統(tǒng)的熱力學(xué)分析[J].武漢工程大學(xué)學(xué)報(bào)(自然科學(xué)版},2009,31(7):912,CUI Guo-xing, WANG Wen-sheng, ZHANG Qi-wei. 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