灵武煤CS2／NMP萃取物的柱层析分离及其馏分的GC／MS分析

室温下用等体积的二硫化碳／N-甲基-2-吡咯烷酮（CS2／NMP）混合溶剂对灵武煤进行超声辐射萃取。依次用正已烷、苯、氯仿和四氢呋喃作为展开剂对萃取物进行柱层析分离,得到馏分F1～F4,用气相色谱／质谱联用仪（GC／MS）分析各馏分。结果表明,烷烃高度富集于F1中,F3中稠环芳烃相对含量最高,F4的主要成分是合氧有机化合物。     

神府煤萃取物组成结构的特征分析

采用苯、甲醇、丙酮、等体积的CS2与丙酮的混合溶剂和四氢呋喃依次萃取神府煤,得到其萃取物E1E5,并采用钌离子催化氧化法氧化各级萃取物,所得氧化产物经重氮甲烷酯化后再进行GC/MS分析,以产物组成结构的差异来推测各级萃取物组成结构的差异。结果表明,神府煤萃取物所得酯化产物的主要成分是烷酸甲酯和烷二酸二甲酯,推测其萃取物中含有大量的烷基芳烃和α,ω-二芳基烷烃;且随着溶剂极性的增强,其萃取物氧化后的酯化产物中,烷酸甲酯和烷二酸二甲酯的碳链长度呈一定的递增趋势,推测神府煤中长链烷基芳烃和α,ω-二芳基烷烃易溶于极性较强的溶剂;在氧化产物中还检测出19种甾烷酸甲酯、萜烷酸甲酯和霍烷酸甲酯,表明神府煤萃取物中含有与芳环相连的甾烷基、萜烷基和霍烷基结构。     

NaOCl水溶液氧化玉米秆粉末水不溶物的GC／MS分析

在超声波辐射下用NaOCl水溶液氧化玉米秆粉末（CSP）,经过滤分离得到滤液和滤渣,依次用CS2、CH3OH和CH3COCH3萃取滤渣,得到萃取物E1～E3,用Gc／Ms分析E1～E3。结果表明,在二硫化碳萃取物中共检测出17种有机化合物,且大部分为有长碳链结构的有机物;在甲醇萃取物中只检测出1种长链脂肪酸酯;在丙酮萃取物中共检测出40种有机物,包括多种芳香族化合物及少量正构烷烃。     

Separation and analysis of lignite bioconversion products

The bioconversion of coal at ambient conditions is a promising technology for coal processing, although the mechanisms of coal degradation are still not understood fully. In this work, the bioconversion of lignite was studied using a fungus isolated from decaying wood. The lignite samples were oxidized with nitric acid under moderate conditions and then the oxidized samples were placed on a potato medium with isolated fungus for lignite bioconversion. Lignite, oxidized lignite and residual products after bioconversion of lignite were sequentially extracted with petroleum ether, CS₂, methanol, acetone and tetrahydrofuran (THF), and then each extract was characterized by gas chromatography–mass spectrometry (GC/MS). The differences in composition and structure among the samples were inferred by comparing the differences between the extracts. The results show that aromatics with one or several benzene rings and their derivatives; and some long-chain alkanes containing oxygen decreased in the methanol-, acetone-, and THF-soluble fraction from residual lignite, whereas long chain or a few branched alkanes and small quantities of aromatic compounds increased in petroleum ether and CS₂ soluble fractions.     

胜利褐煤二硫化碳-丙酮萃取物的超临界醇解物的GC/MS分析

胜利褐煤经CS2-丙酮混合溶剂(V/V=1 1)萃取获得萃取物EM,EM在300℃的甲醇中热溶2 h获得热溶物ET.对EM和ET进行了气相色谱/质谱联用(GC/MS)分析,在EM中有43种GC/MS可检测组分,而在ET中检测到了132种有机化合物,其中包括32种在EM中未检测到的甲酯类化合物(MAs)和16种酚类化合物.分析了MAs和酚类化合物的形成机理,得出了胜利褐煤CS2-丙酮可溶大分子化合物中可能存在的4种结构单元.本文提供了一种研究煤中可溶大分子化合物的有效方法,弥补了GC/MS在检测大分子化合物时的不足.     

微波辐射下麦秆的氧化解聚研究

在微波辐射下通过正交实验研究麦秆在H2O2/丙酮体系中氧化解聚的适宜条件。采用二硫化碳、苯、甲醇、丙酮和四氢呋喃对未氧化和氧化的麦秆进行分级萃取,比较麦秆各级萃取物的相对含量和组成差异,并对各级萃取物的组成进行GC/MS分析。结果表明,麦秆氧化解聚适宜条件是,麦秆量为1.0 g、微波功率为（365±18.25）W、反应时间为20 min。分级萃取可以实现对麦秆中可溶有机质的族组分分离,氧化后麦秆各级萃取物物种数量增多,说明在H2O2/丙酮体系中对麦秆氧化解聚有着明显效果。     

徐州圣戈班高温煤焦油的分离和GC/MS分析

以徐州圣戈班高温煤焦油为原料,在超声辐射下用石油醚（PE）萃取,将煤焦油分离为石油醚可溶物（PESF）和石油醚不溶物（PEIF）。在索氏萃取器中依次用石油醚、甲醇和乙醇萃取PEIF,得到3种萃取物,分别记为E1、E2和E3。用气相色谱/质谱联用仪（GC/MS）分析PESF、E1、E2和E3,在PESF和E1中共检测到235种组分,主要是1-6环芳烃,还有少量含杂原子（氧、氮、硫）的有机化合物,在E2和E3中没有检测出任何化合物。结果表明,以PE为溶剂、通过超声辐射和索氏萃取可以从煤焦油中分离出所有的GC/MS可测成分。     

两种烟煤CS2溶剂分次萃取物的FTIR分析

为揭示煤中可溶组分的存在方式和溶出行为，以CS2为溶剂对两种烟煤进行了约1000h的索氏萃取，按时间段分批（次）提取萃取物进行了FTIR定性和定量分析，结果表明，CS2可萃取组分的溶出具有明显的时序性、阶段性和某些爆发性的特点，波形曲线是萃取物溶出时一些重要基团吸收峰面积随时间变化的典型特征，曲线形状、生波位置、波峰时刻和波幅大小随煤种而不同，2950～2858，3040，1610，860，815，750cm^-1的吸收峰面积和累积萃取时间分别以AR，AAr1，AAr2，AAr3，AAr4，AAr5和t表示，则AR／AAr2～t曲线的波峰所处时刻反映着萃取物中所合脂链的长短，波幅反映着所含脂链成分的数量；AR/AAr1-t,AAr3/AAr1-t,AAr4/AAr1-t和AAr5/AAr1-t曲线的相互结合还指示出单个氢原子、两个相邻氢原子和4个相邻氢原子被取代芳环的溶出行为．脂链和侧链与煤中其它部分形成非共价键时的多点联结是形成波形溶解曲线的重要原因．     

稻壳粉末乙醇解残渣的组成分析

用傅里叶变换红外光谱仪（FTIR）分析稻壳粉末乙醇解残渣,发现残渣富含含氧基团。依次用CS2和等体积的CS2与丙酮的混合溶剂萃取残渣,得到萃取物E1和E2,用气相色谱／质谱联用仪（GC／MS）分析E1和E2,从E1中检测出3种烷烃、苯族烃和萘族烃各5种、2种含硅有机化合物和2-乙氧基四氢呋喃;从E2中检测出2种含氧有机化舍物和5种烃类化合物,其中含氧有机化合物的相对含量比E1中的相应物含量高。     

Separation and analysis of aromatic hydrocarbons from two Chinese coals

Separation and analysis of aromatic hydrocarbons (AHs) from coals is of considerable significance for both fuel and non-fuel use of the coals. In present work two Chinese bituminous coals were selected for separation of AHs by ultrasonic extraction with CS2 followed by column chromatography using hexane as eluent. A series of AHs were separated from the two coals and analyzed by GC/MS. FTIR was employed to characterize the raw coals and the extracted residues. The results of GC/MS analysis show that the separated AHs are mono- to tetracyclic arenes, among which the principle AHs are alkyl naphthalenes and phenanthrenes. Obvious differences in the composition and the structure of AHs exist between the two coals, i.e., the AHs from Tongting coal tend to be higher rings compared to those from Pingshuo coal both from the variety and from the abundance of the AHs. FFIR analysis shows that the raw and extracted coals are similar in terms of functional groups, suggesting that the composition and structure of CS<,2> extract, especially the AHs, from coals can be used to interpret the coal structure to some extent.     

CS2 extraction and FTIR & GC/MS analysis of a Chinese brown coal

The abundance of low-rank coals in China, such as bituminous and brown coals, makes studies of their composition and structure of great significance to both coal chemistry research and for efficient utilization of the coal. We describe how a Chinese brown coal was ultrasonically extracted with carbon disulfide (CS2) and the raw and extracted coals were characterized by Fourier Transform Infrared Spectroscopy (FTIR). The corresponding extract was analyzed with a coupled gas chromatograph mass spectrometer (GC/MS). The FTIR analysis shows a great abundance of amidocyanogen, carbonyl, aromatic and hetero aromatic rings and single carbon-heteroatom bonds. This suggests the possible occurrence of compounds like alcohols, phenols, amines, esters, carboxylic acids, ethers, aromatics or heteroaromatics. The GC/MS analysis of the CS2 extract detected 62 compounds, among which the non-polar ones were of lower abundance while the polar ones were in higher abundance and were structurally diverse. This demonstrates the compositional and structural complexity of Shengli coal.     

氧化钙催化的霍林郭勒褐煤的超临界甲醇解研究

制备用于催化褐煤超临界甲醇解的固体碱CaO,并用XRD和CO2-TPD对其进行表征。分别考察反应温度、时间及CaO和CH3OH的用量对霍林郭勒褐煤解聚反应的影响。依次用CH3OH、等体积的CH3COCH3与CS2混合溶剂、等体积的THF与CS2混合溶剂进行萃取分离,得到萃取物E1、E2和E3,并采用GC／MS对可溶物组分进行分析。结果表明,在反应温度为320℃、CaO用量为0．6g、甲醇用量为20mL、反应时间为2h的条件下,霍林郭勒褐煤醇解的总萃取率可达70％以上;E1中共检测到77种有机化合物,主要是酚类、烷烃类、酮类和含杂原子化合物。     

Effects of coal rank,Fe304 amounts and activation temperature on the preparation and characteristics of magnetic activated carbon

Coal-based Magnetic Activated Carbons(CMAC's)were prepared from three representative coal samples of various ranks:Baorigele lignite from Inner Mongolia; Datong bitumite from Shanxi province; and Taixi anthracite from Ningxia Hui Autonomous Region.Fe3O4 was used as a magnetic additive.A nitrogen-adsorption analyzer was used to determine the specific surface area and pore structure of the resulting activated carbons.The adsorption capacity was assessed by the adsorption of iodine and methylene blue.X-ray diffraction was used to measure the evolution behavior of Fe3O4 during the preparation process.Magnetic properties were characterized with a vibrating-sample magnetometer.The effect of the activation temperature on the performance of CMAC's was also studied.The results show that,compared to Baorigele lignite and Talxi anthracite,the Datong bitumite is more appropriate for the preparation of CMAC's with a high specific surface area,an advanced pore structure and suitable magnetic properties.Fe3O4 can effectively enhance the magnetic properties and control the pore structure by increasing the ratio of mesopores.An addition of 6.0% Fe3O4 and an activation temperature of 880 ℃ produced a CMAC having a specific surface area,an and 4.623 emu/g,respectively.The coal used to prepare this specimen was Datong bitumite.     

GC/MS Analysis of Fractional Extraction of Fusain from Tongting Bituminous Coal in CS2

Fusain from Tongting （Huaibei, Anhui Province） bituminous （FTTB） coal was fractionally extracted using Soxhlet extractor with CS2. Then the extracts were analyzed with GC/MS. Comparison of experimental data between FTTB coal and clarain from Tongting bituminous （CTTB） coal was carried out. The results show that the kinds of small molecule components detected by GC/MS of FTTB are less than those of CTTB. Long-chain alkanes exist mostly in the extracts of fusain. Macromolecular networks are predominant in the FTTB coal mainly composed of inertinite in the coal petrography. The size of micropores in the FTTB coal is relatively small, and the development of micropores is relatively low. Thus the content of aromatic compounds with affinity for micropores is relative low in FTTB, while the content of long-chain alkanes with affinity for macromolecule networks is relatively high. Sub-components in exinite determine the distribution of long-chain alkanes extracted in the last stage. Odd-numbered carbon distribution appears when resin is most in exinite, while high carbon alkane distribution appears when exinite is dominant in cutinite. Small aromatic molecules are firstly packed in micropores, and exist in a free state after micropores are saturated.     

Group separation and analysis of a carbon disulfide-soluble fraction from Shenfu coal by column chromatography

A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four clear group fractions and a nonpolar fraction. All the fractions were analyzed by GC/MS. A total of 204 compounds were detected from the original CDSSF and its further separated fractions, with 173 compounds more than those detected by studying the original CDSSF directly. The results demonstrate a clear group separation by column chromatography in coal organic components and a more accessibility to coal components compared with the solvent extraction only.     

新型吡嗪甲酰-L-苯丙氨酰-L-亮氨腈/缬氨腈二肽的合成

利用混合酸酐法和催化氢化经6步反应,合成了4种新型吡嗪甲酰-L-苯丙氨酰-L-亮氨腈/缬氨腈二肽,对反应条件进行了优化,利用IR、1 H NMR、13 C NMR和HR-MS对其结构进行了表征。结果表明:对于混合酸酐法,反应温度0℃,THF为溶剂,三乙胺为缚酸剂,n(氨基酸)∶n(Et3N)∶n(ClCOOEt)=1∶1.5∶1.5时,缩合反应的产率最高可达90%;对于催化氢化反应,以甲醇为溶剂,10%Pd/C为催化剂,催化剂的质量分数为30%,反应时间为30min时,氢化反应产率最高可达90%。该法原料价廉易得,操作简便,反应条件温和,产率较高。     

Solubilization of small molecules from coal and the resulting effects on the pore structure distribution

The solubilization of small molecules from coal by solvent extraction and the resulting effects on the pore distribution of a low rank coal were studied. Samples were extracted, in succession, with petroleum ether and with CS2. Extract and residue frac-tions collected during the solubilization process were analyzed by FTIR and by surface area and porosimetry. The results show that an obvious inflection point exists that allows separating the dissolution sequence into stages. Small molecules are first extracted from the free state, then molecules trapped in micropores are extracted and, finally, molecules trapped in the coal-matrix network are extracted. This is indicated from the extraction yield curves. Chain-like carbonyl compounds, -OH (or-NH) containing com-pounds that are hydrogen bonded and phenolics dominate the petroleum ether extracts. Chain-like carbonyl components and ether compounds (aliphatic ethers and aromatic ethers) dominate the CS2 extracts. A solvent dissolution mechanism and the effect of small molecule extraction on the pore structure are put forward. Diffusion, dissolution, pore opening, pore shrinking or even col-lapsing caused by swelling, creating of new micropores, pore opening and, finally, colloidallization of some micropores occurs. In the later stages of the extraction the internal structure of the coal is colloidallized due to swelling and the pore number or volume is greatly reduced.     

从四氢呋喃,乙醇,甲醇,水四元混合物系中分离四氢呋喃的研究

以液－液萃取,氧化,间歇精馏为手段,从四氢呋喃,乙醇,甲醇和水四元混合物系中分离四氢呋喃,四氢呋喃的纯度超过９８％,收率超过５８％,本试验选取极性与四氢呋喃相似但沸点相差很大的二甲苯为四氢呋喃的萃取剂,使萃取后二者的分离十分方便,且萃取剂可以复套用,为实际应用提供了可能。     

超细与常规煤粉的热解特性及其热解机理的研究

结合积分法和微分法,由热解曲线和动力学方程出发,得到了适合不同粒度的大同烟煤和元宝山褐煤的热解机理,上述煤种热解反应都遵循Zhuralev,Lesok in和TemPelm an三维扩散方程;同时对大同烟煤和元宝山褐煤不同粒度的煤样的热解特性进行研究,由实验数据得到了热解反应动力学参数,为进一步研究超细和常规煤粉的着火、燃烧提供了理论基础.     

邯郸市区落尘中部分有害成分分析

对邯郸市主要街道落尘成分进行了有机和无机化学成分分析 ,根据化验数据 ,对代表性重金属元素、总有机碳和多环芳香烃等进行了污染状况研究。通过分析结果的对比和印证 ,得出邯郸市区存在着较重的Cu、Hg、Pb和有机物的污染 ,污染源主要为土壤尘和燃煤颗粒