低阶煤在煤液化衍生油中的热萃取性能

以煤液化油衍生油为溶剂,在热萃取装置上研究了大唐胜利褐煤等低阶煤的热萃取性能,考察了热萃取温度、热萃取时间、溶煤比、溶剂类型和煤种等因素对煤热萃取性能的影响,同时对大唐胜利褐煤在热萃取过程中氧元素的脱除情况进行了研究.结果表明:煤的热萃取率随温度升高而明显增加,由340℃时的18.7%(daf)增加到430℃时的59.5%(daf),而固体热萃取物回收率在390℃时达到最高值32.4%(daf),反应停留时间以60 min为宜,溶剂与煤的合适质量比为5∶1,在煤液化加氢循环溶剂中具有较高的热萃取率.热萃取过程中大唐胜利5#煤中氧元素的脱除率可达23%(daf).     

基于COSMO-RS模型的分离油酚混合物的离子液体萃取剂筛选

低温煤焦油中酚类化合物的分离对其充分利用具有重要意义。基于COSMO-RS模型,以间甲酚和异丙苯作为模型化合物,研究了离子液体在分离油酚体系中的应用;利用Turbomole软件建立了包含27种离子液体阴离子和48种离子液体阳离子的s-图谱数据库,结合COSMOtherm软件对组成的1296种离子液体进行筛选,探讨了阴阳离子对间甲酚分离效果的影响,并对筛选得到适宜的离子液体进行液液相平衡实验验证。结果表明,离子液体阴离子对间甲酚分离效果影响较大,以Cl^-和CH₃COO^-为阴离子的离子液体与间甲酚之间具有较强的氢键相互作用,因此具有较好的分离效果;阳离子对间甲酚分离效果影响较小,碳链或支链的增加能适当提高离子液体对间甲酚的分离效果。实验得到的bmimOAc、bmimCl、emimOAc、TPAC四种离子液体-间甲酚-异丙苯的液液相平衡数据表明,四种离子液体对间甲酚均具有较大的分配系数和选择性,且萃取分离效果的顺序为：emimOAc > bmimOAc > TPAC > bmimCl,与COSMO-RS模拟筛选得到的结果一致,表明筛选具有较高的准确性。     

超声萃取中低温煤焦油轻质油中酚类化合物研究

针对陕北榆林地区中低温煤焦油利用率低、环境污染严重等问题,以陕北榆林地区中低温煤焦油轻质油为原料,丙三醇水溶液为萃取剂,采用超声萃取法萃取中低温煤焦油轻质油中的酚类化合物,考察丙三醇添加量、丙三醇水溶液质量分数、超声温度等工艺条件对酚类化合物萃取率的影响。结果表明,丙三醇添加量对萃取结果影响最大,其次是丙三醇水溶液质量分数,超声温度对萃取结果的影响较小。最佳萃取条件为:丙三醇与轻质油质量比3.5∶1,丙三醇水溶液质量分数25%,萃取温度55℃,超声频率25 k Hz,酚类化合物萃取率高达93.9%。     

煤炭直接液化油中酚类化合物的分离与利用

酚类化合物是煤炭直接液化产物中具有较高附加值的主要含氧化合物,也是煤液化油酸性物质的主要成分。它不仅对油品的提质加工的技术路线有影响,而且也对煤炭直接液化的经济性具有较大的影响。由于该方面的研究工作尚属起步阶段,借鉴煤焦油和石油系产品中酚类化合物的有关分离与利用情况,结合笔者的研究实践和认识,提出了在煤直接液化油中酚类的分离与利用方面应开展的工作和研究方向。     

基于分子模拟的低温煤焦油中酚类化合物的溶解特性

低温煤焦油中酚类化合物溶解行为及机理研究是其高效分离的基础。本文以焦油中的典型组分为研究对象,借助混合能参数,模拟计算各组分与酚类化合物的相溶性;在焦油模型中,借助相互作用能、径向分布函数计算及电子密度分析,探究酚类化合物的溶解机理。结果表明：①焦油中各组分物质苯环上取代基基团、苯环数量等结构特征是影响酚类化合物在焦油中溶解行为的关键;②酚类化合物在各组分中的溶解行为受到缔合作用的影响,缔合作用越大、空间位阻效应越小,酚类化合物与其他组分相溶性越强;③模型焦油中,苯酚与苯、苯并噻吩之间缔合作用力均为π-π堆积作用力,苯酚与正己烷、吲哚之间缔合作用力分别为CH-π堆积作用力和N—H···O氢键。     

Effect of various extraction conditions on the phenolic contents of pomegranate seed oil

Pomegranate seeds are byproducts of the pomegranate juice industry. Because of the presence of large amounts of certain pharmaceutical and nutraceutical components in the seeds, a proper extraction method to obtain these components is highly demanded in the food industry. In this study, the effect of different extraction methods on the total phenolic contents of the oil extracted from pomegranate seeds of the Malas variety from Shahreza, Iran, was investigated. Four different extraction methods including normal stirring, Soxhlet, microwave irradiation and ultrasonic irradiation using two types of organic solvents as well as a supercritical fluid extraction (SFE) method using CO₂ as solvent were applied. The different organic solvents of this study did not indicate any significant differences in the total phenolic contents of the extracted oils, but the extracted oils from the various conditions of SFE indicated wide changes in the amount of phenolic compounds (7.8–72.1 mg/g). The total phenolic content of the extracted oil from one of the SFE runs was several times greater than those in the extracted oils using organic solvents.     

煤与油页岩热预处理特性及对热解的影响

对比研究了神木煤和桦甸油页岩在150~400℃热预处理时的孔隙变化和挥发分析出规律以及热预处理对后续慢速升温热解反应产物的影响。结果表明,热预处理显著增加了油页岩的孔隙结构,其比表面积提高4倍、孔体积提高5倍以上,而神木煤的孔隙结构则减少了,特别是孔径大于1 nm的孔体积减少了近60%、比表面积减少了近80%,而其1 nm以下的孔则相对稳定,孔体积和比表面积分别只减少了10%左右。低于400℃时热预处理过程中除脱去吸附水外,其他挥发分也有一定析出,并以CO₂为主,另有少量CO,但挥发分总失重量不超过5%。固定床慢速升温热解研究表明,经热预处理后,油页岩的油产率最高提高了22.7%,而水和气的产率则相应降低,气体中CH₄增加而H₂降低。热预处理对煤的热解油产率影响不明显,但热解水产率降低而热解气产率增加且其中CH₄增多而H₂降少。     

复合添加剂对石煤提钒焙烧与浸出工艺研究

利用复合添加剂焙烧、低浓度酸浸出法对石煤矿进行提钒研究,考察了焙烧、浸出两个过程中各种工艺参数对浸出率的影响。实验结果表明,适宜的焙烧、浸出工艺条件为:复合添加剂中添加剂硫酸钠、氯化钠、碳酸钠的最佳质量比为7∶1∶11,焙烧温度为750℃,焙烧时间为2.5 h,浸出温度为50℃,浸出时间为5 h。最佳工艺条件下钒的浸出率可达81.9%,明显高于传统的钠法焙烧工艺。     

基于显微组分化学键特征的宁夏庆华煤热解特性及动力学分析

通过X射线光电子能谱和傅里叶红外光谱表征宁夏宁东庆华煤不同显微组分的官能团种类、表面结构元素价态分布及化学键赋存特征。采用热重-质谱联用考察庆华煤镜质组和惰质组在不同热解温度下的失重行为和关键气体组分变化。进一步基于Coats-Redfern模型从化学键断裂特征和反应动力学角度探讨煤镜质组和惰质组的热解行为差异。结果表明,庆华煤显微组分的热解失重峰与相应化学键断裂信息能够很好地吻合。不同显微组分的热重曲线变化趋同,但相同热解温度下镜质组的失重率始终高于惰质组。快速热解阶段镜质组较惰质组表现出更大的失重率和最大失重速率。其主要原因在于镜质组的脂肪族官能团相对含量更高,快速热解阶段会发生更多的C_al—C_al断裂。不同热解温度下庆华煤显微组分三个主要热解阶段的活化能和频率因子大小次序为：快速热解阶段>快速缩合阶段>缓慢热解阶段。在快速热解阶段,镜质组和惰质组的平均活化能均约为75 kJ/mol,但镜质组的频率因子更高。     

Hydrotreatment of heavy oil from a direct coal liquefaction process on sulfided Ni-W/SBA-15 catalysts

A series of Ni-W catalysts supported on SBA-15 with different pore sizes were prepared by incipient wetness impregnation method and characterized by N₂ adsorption-desorption and X-ray diffraction. The hydrogenation of heavy oil (distillation temperature: 320-340 °C) derived from the direct coal liquefaction process using Shengli coal in the presence of sulfided Ni-W/SBA-15 catalysts with different pore sizes were evaluated at 400 °C and initial H₂ pressure of 5.0 MPa. The results showed that the catalyst preparation method and the pore size of the support had a significant influence on the Ni/W crystallite size, hydrodenitrogenation (HDN) and hydrodearomatization (HDA) activities of coal-derived heavy oil. The larger pore could cause the Ni-W/SBA-15 to form larger Ni-W crystallite. The catalysts with largest pore in the range studied displayed highest HDN and HDA activities for upgrading of the coal-derived heavy oil.     

The effect of extraction techniques on yield,extraction kinetics,and antioxidant activity of aqueous-methanolic extracts from nettle (Urtica dioica L.) leaves

Five extraction techniques, maceration, reflux, Soxhlet, Tillepape, and ultrasonic extraction, were used to obtain the extractive matter from nettle leaves. The antioxidant activity of extracts was assessed by DPPH, FRAP, and H₂O₂ test, while the total phenolic and total flavonoid content was determined according to the Folin–Ciocalteu and aluminium chloride methods, respectively. Model Ponomarev and a non-stationary diffusion model through the plant material were used for modelling extraction process. The extract obtained by Soxhlet extraction, containing higher amounts of extractive matter as well as phenolic and flavonoid compounds, showed better antioxidant activity than those obtained by other extraction techniques.