化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2014年
11期
4383-4391
,共9页
周奕杉%陈利平%陈网桦%杨庭%张彩星%尹瑞丽
週奕杉%陳利平%陳網樺%楊庭%張綵星%尹瑞麗
주혁삼%진리평%진망화%양정%장채성%윤서려
安全%稳定性%动力学%TD24%一硝基甲苯%差示扫描量热%绝热量热
安全%穩定性%動力學%TD24%一硝基甲苯%差示掃描量熱%絕熱量熱
안전%은정성%동역학%TD24%일초기갑분%차시소묘량열%절열량열
safety%stability%kinetics%TD24%mononitrotoluene%differential scanning calorimetry%adiabatic calorimetry
为获取甲苯一段硝化未经碱洗产物(样品1:一硝基甲苯+少量混酸)及碱洗后的纯品产物(样品2:一硝基甲苯)在绝热条件下最大温升速率达到时间为24 h所对应的引发温度TD24,并了解其热分解特性,首先采用差示扫描量热仪(DSC)测试了两种样品不同升温速率下的动态DSC数据,分析获得了样品的机理函数、活化能和指前因子,进而推导出两个样品的TD24分别为(246.1±4.5)℃和(257.9±3.6)℃。然后利用绝热加速度量热仪(ARC)对此进行了实验验证,得到绝热条件下样品1和2的TD24分别为241.5℃和256.4℃。上述结果表明,DSC推导的TD24结果与ARC结果几乎一致。这表明根据动态DSC测试参数推导的TD24具有一定的可靠性,可以作为工程应用的参考;就甲苯一段硝化产物而言,含酸体系的热分解危险性更高。
為穫取甲苯一段硝化未經堿洗產物(樣品1:一硝基甲苯+少量混痠)及堿洗後的純品產物(樣品2:一硝基甲苯)在絕熱條件下最大溫升速率達到時間為24 h所對應的引髮溫度TD24,併瞭解其熱分解特性,首先採用差示掃描量熱儀(DSC)測試瞭兩種樣品不同升溫速率下的動態DSC數據,分析穫得瞭樣品的機理函數、活化能和指前因子,進而推導齣兩箇樣品的TD24分彆為(246.1±4.5)℃和(257.9±3.6)℃。然後利用絕熱加速度量熱儀(ARC)對此進行瞭實驗驗證,得到絕熱條件下樣品1和2的TD24分彆為241.5℃和256.4℃。上述結果錶明,DSC推導的TD24結果與ARC結果幾乎一緻。這錶明根據動態DSC測試參數推導的TD24具有一定的可靠性,可以作為工程應用的參攷;就甲苯一段硝化產物而言,含痠體繫的熱分解危險性更高。
위획취갑분일단초화미경감세산물(양품1:일초기갑분+소량혼산)급감세후적순품산물(양품2:일초기갑분)재절열조건하최대온승속솔체도시간위24 h소대응적인발온도TD24,병료해기열분해특성,수선채용차시소묘량열의(DSC)측시료량충양품불동승온속솔하적동태DSC수거,분석획득료양품적궤리함수、활화능화지전인자,진이추도출량개양품적TD24분별위(246.1±4.5)℃화(257.9±3.6)℃。연후이용절열가속도량열의(ARC)대차진행료실험험증,득도절열조건하양품1화2적TD24분별위241.5℃화256.4℃。상술결과표명,DSC추도적TD24결과여ARC결과궤호일치。저표명근거동태DSC측시삼수추도적TD24구유일정적가고성,가이작위공정응용적삼고;취갑분일단초화산물이언,함산체계적열분해위험성경고。
To determine the temperature of sample 1 (toluene mono-nitration crude product: mononitrotoluene with a little mixed acid) and sample 2 (pure mononitrotoluene product, MNT)TD24, at which the required time to reach maximum rate of temperature rise under adiabatic condition is 24 hours, and to obtain the thermal decomposition characteristics of these products, differential scanning calorimeter (DSC) and accelerating rate calorimeter (ARC) were employed to test the thermal behaviors of the two samples. By kinetic analysis for dynamic data obtained by DSC in dynamic mode, theTD24 determined for samples 1 and 2 are (246.1±4.5)℃ and (257.9±3.6)℃, respectively. As a comparison, the values ofTD24 for sample 1 and 2, determined by ARC under adiabatic condition, are 241.5℃ and 256.4℃, respectively. Therefore, theTD24 values derived from dynamic data are in good agreement with those by ARC, which means that the results derived from DSC are of large reliability and can be used as a reference for engineering applications. Meanwhile, a comparison for the results of sample 1 and 2 indicates that the thermal hazard of MNT with a little mixed acid is higher than that of pure one.