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Comparative studies on the structural features of soluble portions from thermal dissolution/methanolysis and catalytic hydroconversion of an extraction residue from Heishan lignite

机译:黑山褐煤提取残渣热解/甲烷分解及催化加氢转化可溶部分结构特征的比较研究

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Heishan lignite (HL) was extracted with isometric acetone/carbon disulfide mixed solvent under ultrasonic irradiation. The extraction residue (ER) was subjected to thermal dissolution/methanolysis (TD/M) in methanol and catalytic hydroconversion (CHC) in cyclohexane (CH) at 300 degrees C under 1 MPa of N-2 over a supported acid (SA). The methanol-soluble portion (MSP) from the TD/M and CH-soluble portion (CHSP) from the CHC were analyzed with a gas chromatograph/mass spectrometer (GC/MS) and Fourier transform infrared (FTIR) spectrometer, while ER and the residues from the TD/M (R-TD/M) and CHC (R-CHC) were characterized with the FTIR spectrometer and an X-ray photoelectron spectrometer (XRPES). The results show that the yields of MSP and CHSP are ca. 22.6% and 16.1%, respectively. According to the analysis with GC/MS, CHSP is rich in tetra-methylbenzenes and dimethylnaphthalenes, while most of the GC/MS-detectable compounds in MSP are xylenols, trimethylphenols, and methyl normal alkanoates. During the TD/M, the cleavage of some C-O bonds could be the main reaction, whereas the SA effectively catalyzed the cleavage of C-ar-C-alk bonds connecting some aromatic rings (ARs) and side chains on the ARs in ER. No significant difference in the distribution of functional groups was observed in FTIR spectra between HL and ER, while the distribution of functional groups in MSP is extraordinarily different from that in CHSP. According to the analysis with XRPES, RTD/M has higher carbon content but lower oxygen content.
机译:在超声辐射下,用等量丙酮/二硫化碳混合溶剂萃取黑山褐煤(HL)。将萃取残留物(ER)在甲醇中进行热溶解/甲烷水解(TD / M),然后在300℃,1 MPa N-2压力下,在负载酸(SA)上在环己烷(CH)中进行催化加氢转化(CHC)。使用气相色谱/质谱仪(GC / MS)和傅立叶变换红外(FTIR)光谱仪分析TD / M的TD / M甲醇可溶部分(MSP)和CHC的CH可溶部分(CHSP),而ER和用FTIR光谱仪和X射线光电子能谱仪(XRPES)对TD / M(R-TD / M)和CHC(R-CHC)的残留物进行表征。结果表明,MSP和CHSP的产率约为。分别为22.6%和16.1%。根据GC / MS的分析,CHSP富含四甲基苯和二甲基萘,而MSP中大多数可通过GC / MS检测到的化合物为二甲苯酚,三甲基苯酚和正链烷酸甲酯。在TD / M过程中,某些C-O键的断裂可能是主要反应,而SA有效催化了ER中连接芳族环(AR)和AR侧链的C-ar-C-烷键的断裂。在HL和ER之间的FTIR光谱中,观察到的官能团分布没有显着差异,而MSP中的官能团分布与CHSP中的官能团分布极为不同。根据XRPES的分析,RTD / M的碳含量较高,但氧含量较低。

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