微波条件下氯化锌对乙醇抽提神府煤的影响

微波条件下,研究了在乙醇抽提神府煤中加入氯化锌对其结果的影响。采用气相色谱/质谱联用的方法分析了乙醇和乙醇-氯化锌抽提物的组成;利用傅里叶红外光谱技术分析了神府脱矿物质煤、乙醇抽余煤和乙醇-氯化锌抽余煤的结构。分析结果显示:在乙醇溶剂中添加少量的氯化锌,其抽提物的组成发生了改变;乙醇-氯化锌抽余煤与原脱矿物质煤和乙醇抽余煤相比,芳环吸收强度降低,表明在抽提过程中可能伴随着烷基化反应的发生。     

吡啶抽提前后柳林3~#煤的FTIR结构特征分析

为了解处于第二次煤化跃变过程中的柳林3~#煤的大分子结构特征,采用溶剂吡啶对柳林3~#原煤进行索氏抽提,借助FTIR分析测试手段并通过分段分峰拟合对柳林3~#原煤、抽提后残煤及抽提物的结构组成及其变化进行了研究。结果表明:抽提过程中,在吡啶溶剂的作用下,部分抽提物从煤大分子结构中脱离出来,这些抽提物包括短链脂肪结构和芳香醚、酚、酯等含氧官能团结构。抽提前后煤大分子骨架保持相对稳定,与原煤和抽提后残煤相比,抽提物的苯环四取代明显增加,二取代明显减少,说明残煤的脂肪链长、支链少,抽提物的脂肪链短、支链多。抽提后残煤、抽提物与原煤显示出不同的芳香度,其由大到小依次为抽提后残煤的芳香度、原煤的芳香度、抽提物的芳香度;柳林3~#原煤、抽提后残煤及抽提物中主要羟基类型是自缔合羟基,说明煤中羟基类型以缔合结构为主。     

微波辅助抽提煤的实验研究

在微波辅助下,以四氢呋喃、乙醇和乙酸为溶剂抽提神府煤,考察了抽提温度、抽提时间、溶剂用量及煤粒度对抽提率的影响;同时探讨了上述三种溶剂对不同变质程度的攀枝花煤、铜川煤、神府煤、华亭煤和依泰煤在微波辅助下的抽提效果.结果表明,抽提率在一定的抽提温度、时间、溶剂用量及煤粒度下均有最佳值;变质程度相似的煤在相同抽提条件下抽提率不同.运用红外光谱现代分析技术,对神府脱灰煤和其抽提残煤的结构特征进行了对比分析,结果表明,抽提并没有破坏煤的大分子结构;利用GC/MS测定了铜川煤的乙醇微波辅助抽提物的组成.     

利用红外光谱研究黄陵烛煤溶剂抽提产物

为开发黄陵烛煤在制取化学品和高性能材料的新工艺方面的应用,在探索适宜于黄陵烛煤溶剂抽提体系的基础上,运用红外光谱现代分析技术,对原煤和不同溶剂中抽提得到的残煤的组成和结构特征进行对比分析;并分析所得到的抽提物,得出烛煤的芳香度很低,芳环数少,残煤主要富集的是含芳环结构的成分和矿物质,而抽提物以脂肪结构物质为主．     

煤的CS2/NMP混合溶剂抽提研究进展

综述了 CS2 /NMP混合溶剂用于煤抽提的研究进展 ,着重介绍了煤阶、煤岩组分、添加物和各种辅助手段对抽提率的影响 ,并对添加物的增溶机理、混合溶剂的抽提机理、抽提动力学以及抽提物的表征等问题进行了讨论 ,指出高抽提率的溶剂抽提不仅对于煤结构的研究有着重要的意义 ,而且可望成为获取高附加值产品和煤净化的新途径     

不同溶剂抽提下高阶煤的化学组成和结构变化

以山西长治霍尔辛赫矿贫煤为研究对象,对煤样分别进行了不同溶剂的抽提,并借助柱层析法和X射线衍射技术(XRD)对抽提物和抽余物进行了测试分析.结果表明:高阶煤进行溶剂抽提后,THF对煤样的抽提率最高,其次是CS2、丙酮和乙醇,苯的抽提率最低;除CS2抽提物中非烃类含量高于总烃含量外,其余溶剂的抽提物均表现为总烃含量大于非烃类含量,同时,随着抽提效果的增强,抽提物中非烃类化合物的质量分数逐渐增大;经溶剂抽提后抽余物的基本结构单元(BSU)的芳香层间距d002、堆砌度Lc和芳香层数N均表现出大于原煤微晶结构的规律,而延展度La在溶剂抽提后却呈现出小于原煤微晶结构延展度的特性.     

溶剂类型对煤微波辅助抽提率及组成的影响

以神府煤和攀枝花煤为对象进行煤微波辅助抽提研究,所用溶剂有甲醇、乙醇、丙酮、乙酸、四氢呋喃、乙二胺和DMF等.结果表明,前四种溶剂对攀枝花煤的抽提率较高,后三种溶剂对神府煤的抽提率较高,其中乙二胺对神府煤的抽提率可达70.76%.抽提残煤的元素分析、官能团测定及FT-IR分析表明,各残煤H/C和O/C比略有降低而N/C明显升高;含氧官能团含量较脱灰煤有所增加,总酸性基及羟基含量提高;另外,利用GC/MS检测脱灰神府煤四氢呋喃抽提物,正己烷可溶物含较多的脂肪烷烃,甲苯可溶物中则含各种芳香族化合物,四氢呋喃可溶物中只检测到一种含氧杂原子化合物.     

肥煤的热抽提及其抽提物的性能研究

主要考察了肥煤在不同温度及不同溶剂下的热抽提性能,并对热抽提物性质进行了分析。实验结果表明,提高热抽提温度,肥煤热抽提率增大,并在其软化点附近达到最高值,而后随温度的升高而降低;增大溶剂极性,肥煤热抽提率也显著升高。热重和红外分析显示了热抽提物结构的变化,其基本无灰的特点有望成为煤洁净利用的突破口。     

煤的化学族组成研究(Ⅱ)煤的可溶化体系的优化

煤的可溶化体系是煤化学族组成研究的前提和关键，通过从高抽提率、溶剂回收性、普遍适应性、快捷省时、方便准确等方面综合考察溶剂选择、溶剂组合方式、溶剂抽提方式等因素对煤可溶化的影响，提出了一套较为优化的可溶化体系，以满足煤化学族组成研究的需要．     

微波辅助下从泥炭中提取黄腐酸类物质的研究

在微波辅助下,以泥炭为研究对象,水为抽提溶剂,采用正交试验考察了抽提温度、时间、固液比及压力对黄腐酸类物质（泥炭水溶酸性抽提物）提取率的影响。结果显示,影响抽提率最主要的因素是压力。较佳的抽提条件为压力0.6MPa、抽提温度150℃、固液比1：10g／ml）、抽提时间20min,并采用红外光谱、元素分析及官能团测定的方法分析了抽提物的组成。采用微波辅助法从泥炭中提取医用黄腐酸可能为一种有效的环境友好的方法。     

煤液化油中酚类化合物分布特征研究

采用气相色谱/质谱联用研究分析了胜利褐煤在0.1t/d直接液化连续实验装置上所得煤液化油中酚类化合物的分布特征.实验通过碱液洗涤法富集煤液化油中混合酚组分,并对该组分进行衍生化处理,以提高色谱柱对混合物的分离性能.以混合衍生物为主要分析对象,共定性出煤液化油中134种个体酚,分属于苯酚、茚满酚、萘满酚和萘酚等四种类型,且绝大多数酚类化合物都带有烷基侧链.苯酚类化合物数量最多,在混合酚组分中含量最大,其次为茚满酚和萘满酚.萘酚类化合物的数量最少,相对含量最小.     

Analysis of solvent extracts from coal liquefaction in a flowing solvent reactor

Point of Ayr coal has been extracted using three solvents, tetralin, quinoline and 1-methyl-2-pyrrolidinone (NMP) at two temperatures 350 and 450 °C, corresponding approximately to before and after the onset of massive covalent bond scission by pyrolysis. The three solvents differ in solvent power and the ability to donate hydrogen atoms to stabilise free radicals produced by pyrolysis of the coal. The extracts were prepared in a flowing solvent reactor to minimise secondary thermal degradation of the primary extracts. Analysis of the pentane-insoluble fractions of the extracts was achieved by size exclusion chromatography, UV-fluorescence spectroscopy in NMP solvent and probe mass. With increasing extraction temperature, the ratio of the amount having big molecular weight to that having small molecular weight in tetralin extracts was increased; the tetralin extract yield increased from 12.8% to 75.9%; in quinoline, increasing extraction temperature didn't have an effect on the molecular weight of products but there was a big increase in extract yield. The extracts in NMP showed the enhanced solvent extraction power at both temperatures, with a shift in the ratio of larger molecules to smaller molecules with increasing extraction temperature and with the highest conversion of Point of Ayr coal among these three solvents at both temperatures. Solvent adducts were detected in the tetralin and quinoline extracts by probe mass spectrometry; solvent products were formed from NMP at both temperatures.     

两种贵州煤苯-甲醇萃取物族组成分析与萃取动力学探讨

利用苯-甲醇混合溶剂对贵州月亮田和六枝2种煤样进行了索氏萃取,并用柱色谱对萃取物进行了族组分分离。利用GC／MS分析研究了萃取物的族组成,并对萃取动力学特征进行了探讨。实验结果表明:萃取过程阶段性明显,萃取物中烷烃和芳烃含量较高;六枝煤中含有多种含氮和含硫的杂环化合物。     

Toluenediamine in polyurethane foams Hazard or artefact?

Abstract

The aim of this study was to investigate the formation of the suspected carcinogen toluenediamine (TDA) as a degradation product of polyurethane. For this purpose, a series of model systems was prepared, including linear polyurethanes and foams. The starting materials were fully characterised using melting point and refractive index determination, end group analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy and coupled gas chromatography–mass spectrometry (GC–MS). A model commercial polyurethane foam was also prepared. Three different solvent extraction protocols were applied and the extracts analysed by coupled GC–MS and high performance liquid chromatography–mass spectrometry. No detectable amounts of TDA could be found in extracts of both linear polyurethane and foam incubated using either toluene or 1% acetic acid solution. By contrast, TDA was found in extracts from both linear polyurethane and foam that had been exposed to alkaline conditions during the extraction procedure. These findings confirm that the formation of TDA in extraction and GC–MS analysis of polyurethane samples results from hydrolytic degradation processes of polyurethane and that alkaline conditions should be avoided during extraction and analysis.     

Rosmarinus Officinalis Leaves as a Natural Source of Bioactive Compounds

In an extensive search for bioactive compounds from plant sources, the composition of different extracts of rosemary leaves collected from different geographical zones of Serbia was studied. The qualitative and quantitative characterization of 20 rosemary (Rosmarinus officinalis) samples, obtained by microwave-assisted extraction (MAE), was determined by high performance liquid chromatography coupled to electrospray quadrupole-time of flight mass spectrometry (HPLC–ESI-QTOF-MS). The high mass accuracy and true isotopic pattern in both MS and MS/MS spectra provided by the QTOF-MS analyzer enabled the characterization of a wide range of phenolic compounds in the extracts, including flavonoids, phenolic diterpenes and abietan-type triterpenoids, among others. According to the data compiled, rosemary samples from Sokobanja presented the highest levels in flavonoids and other compounds such as carnosol, rosmaridiphenol, rosmadial, rosmarinic acid, and carnosic acid. On the other hand, higher contents in triterpenes were found in the extracts of rosemary from Gložan (Vojvodina).     

童亭亮煤索氏萃取和超声萃取的GC/MS分析

采用CS<,2>对童亭亮煤进行索氏萃取和超声萃取,用气相色谱/质谱联用仪(GC/MS)对相关萃取物进行分析,结果表明:童亭亮煤的索氏萃取物由正构烷烃和芳烃构成,而超声萃取物还检测到异构烷烃和各类杂原子化合物,并且随着超声萃取时间的增加,所检测到的物质种类更多结构也更复杂;而超声波的空化效应产生的冲击流能促进溶剂和煤样的...     

山西寺河不同煤体结构煤萃取后的族组成特征

以山西沁水盆地寺河矿无烟煤为研究对象,采用溶剂萃取法,对四类不同煤体结构的煤样分别用苯、四氢呋喃(THF)和1-甲基-2-吡咯烷酮(NMP)溶剂进行萃取,结合柱层析法,对煤样萃取物进行了族组成分析.研究发现,随煤体结构破坏程度的增加,煤样的溶剂萃取率增大.其中NMP溶剂的萃取率最大,THF次之,苯溶剂萃取率最小;随着煤体结构破坏程度的增高,萃取物中的族组成呈现总烃的含量相对下降、非烃类化合物含量总体增加的变化规律.其中,饱和烃类含量减少,芳香烃含量和非烃含量相对增加,而沥青质组分的相对含量减少.     

煤的溶剂抽提规律及其产物性能的研究进展

阐述了温和条件下煤的溶剂抽提机理，煤分子间作用力，溶剂种类对抽提率的影响。抽出物的洁净性能，抽余物的吸附性能，抽提产物表面的物化以及表面活性剂对煤的亲水/疏水性，ζ电位和氮气吸附性能的影响。结果表明，对于高阶煤，加入中性活性剂TericG12A8可以有效降低其ζ电位，增大其氮气吸附量和疏水性。     

Volatilization Loss of 6 PAHs with 2–4 Rings Related to Coal Extracts

ABSTRACT

With 3 different bottles, the volatilities of 6 polycyclic aromatic hydrocarbons (PAHs), namely, acenaphthylene, acenaphthene, fluorene, phenanthrene, fluoranthene and pyrene, which were used as model compounds of coal here, had been measured by using gas chromatography/mass spectrometer (GC/MS). The results indicate that although these PAHs have a high boiling point (BP), some PAHs such as acenaphthylene and acenaphthene can be lost rapidly through volatilizing. Even pyrene, having a BP as high as 404°C, can also be lost by volatilizing for a longer period, such as 4 days or more. The volatilization loss of the PAHs is also related to the container. PAHs in wide-mouthed bottles will volatilize faster than in narrow-mouthed bottles. The volatilization loss of the PAHs and other compounds may lead to incorrect results in quantitatively analyzing them in coal extraction, if coal extracts are dried. So, the coal extracts by organic solvents should not be dried before measuring by GC/MS.     

Solvent degradation during coal liquefaction in a flowing-solvent reactor

We have previously observed that primary coal extracts recovered from the flowing solvent reactor appeared to be of large molecular mass. Short residence times in the reaction zone following the solubilisation of the extracts tended to limit their thermal degradation. This observation offered the vista of detailed characterisation and analysis of most (∼80-90%) of the coal mass in solution-and in a state relatively free of thermal degradation. Point of Ayr coal was extracted with tetralin and with non-donor solvents, quinoline and NMP at 350 and 450 °C. Structural evaluations have been carried out using size exclusion chromatography, UV-fluorescence spectrometry, GC-MS and probe-MS. Little coal derived material could be found in the pentane-soluble part of the reaction mixture; solvent dimers and trimers were prominent and coal-derived components, such as alkanes, were only minor components. In attempting to characterise the main, pentane-insoluble fraction of the coal extract, the level of interference from solvent-derived material emerged as the decisive parameter for the success or failure of the general method. However, the predominantly pentane-insoluble coal extracts from each solvent were contaminated by solvent polymerisation products. For all three solvents, the level of contamination of extracts with solvent derived material tended to interfere with the detailed characterisation/analysis of material extracted from the coal.