第40卷第6期燃料化學(xué)學(xué)報Vol 40 No 6ournal of Fuel Chemistry and TechnologyJun,2012文章編號:0253-2409(2012)060655405煤直接液化殘渣及其萃取產(chǎn)物的熱重分析劉朋飛12,張永奇,房倚天(1.中國科學(xué)院山西煤炭化學(xué)研究所,山西太原03001;2.中國科學(xué)院研究生院,北京10009)摘要:利用熱天平考察了神華和勝利兩種典型中國煤直接液化殘渣及其萃取產(chǎn)物的失重曲線。實驗表明神華殘渣和勝利殘渣的輕質(zhì)組分含量相近其失重率也相近但輕質(zhì)組分組成不同使得失重過程并不一致。升溫速率增加熱解最大失重速率增加,最大失重速率溫度升高。以殘渣各組分失重曲線擬合得到的殘渣失重曲線可近似表示殘渣的失重曲線。動力學(xué)分析表明,由實驗數(shù)據(jù)擬合的活化能和指前因子計算得到的失重曲線,與實際實驗得到的失重曲線較為一致。液化殘渣在低溫區(qū)失重率很高,而且這部分失重產(chǎn)物可以通過溶劑萃取的方式得到。關(guān)鍵詞:煤直接液化;殘渣;熱重;萃取;活化能;指前因子中圖分類號:0643文獻(xiàn)標(biāo)識碼:ATG analysis of coal direct liquefaction residue and its solvent extractsLIU Peng-fei, ZHANG Yong-qi, FANG Yi-tian(1. Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;2. Graduate University of Chinese Academy of Sciences, Bejing 100049, China)Abstract: Pyrolysis of two typical Chinese coal liquefaction residues( Shenhua and Shengli)and their solventextracts was carried out by TG. The results show that Shenhua and Shengli residue contain similar content oflight component, and their weight losses in TGA are similar. However, the different composition of lightcomponent in the two residues leads to their difference in TG curves. As increasing of heating rate, the maximumweight loss rate and its corresponding temperature increase. The calculated weight loss calculated from theconstitutes is approximately the actual value of the residue. From the kinetic analysis, it is found that the weightloss calculated by the experimental E and k, agree well with that obtained from the experiment. The weight lossis mainly caused by evaporation of volatile matter which can be extracted by solventKey words: coal direct liquefaction; residue; thermogravimetric analysis; extract; activation energy; frequency煤直接液化技術(shù)是解決中國未來能源緊張問題1實驗部分的關(guān)鍵技術(shù)之一。煤直接液化殘渣是煤加氫直接液1.1實驗物料及分析方法本實驗所用神華煤液化過程產(chǎn)生的副產(chǎn)品,其產(chǎn)量約占直接液化原煤質(zhì)化殘渣(SHR)取自上海6t/d直接液化中試裝置量的30%左右,殘渣的高效利用直接影響著煤直接勝利煤液化殘渣(SLR)取自煤科總院0.ItUd直接液化工藝過程的經(jīng)濟(jì)性。神華直接液化工廠的液化裝置。兩種殘渣粒徑均小于100目,并在恒溫建成投產(chǎn),標(biāo)志著中國成為世界上掌握百萬噸級直干燥箱中70℃下干燥24h。接液化技術(shù)的國家,但因此產(chǎn)生的大量液化殘渣也利用索氏抽提裝置將液化殘渣分別依次用正己使得液化殘渣的有效處理成為緊迫的問題。烷、甲苯、四氫呋喃萃取,得到的萃取物和最終不溶液化殘渣中含有大量較高經(jīng)濟(jì)價值的重質(zhì)液物在常溫下都為固體索氏提取流程見圖體(2),通常情況下可以采用熱解23的方式將這部熱重分析在 SETARAM熱天平上進(jìn)行。熱解分重質(zhì)液體提取出來加以利用。而萃取是提取殘渣條件為樣品質(zhì)量為6~8mg,N2流量120mL/min重質(zhì)液體的重要手段之一,相比熱解方法其條件也升溫速率為5、10、20、40K/min,終溫為80℃。更加溫和。本實驗將對殘渣及殘渣萃取物進(jìn)行熱重殘渣的工業(yè)、元素分析及溶劑萃取組成見表1。行為研究探討萃取工藝?yán)脷堅刭|(zhì)液體的可行1.2反應(yīng)速率分析性,并得到殘渣的熱解動力學(xué)參數(shù)。E熱重轉(zhuǎn)化率x由式(1)定義中國煤化工CNMHG收稿日期:201140812;修回日期:201114聯(lián)系作者:張永奇,Tel/Fax:0351-2021137,E-mal:zhangye@sice.ac.cn。燃料化學(xué)學(xué)報第40卷其中,α為一定溫度下殘渣揮發(fā)性物質(zhì)的失重對式(6)兩邊取自然對數(shù),且由通常情況下RT