煤基费托合成油中微量总铁的测定

铁系催化剂的残留污染一直是煤间接液化技术生产费托合成油工艺生产和产品质量控制的重点关注问题之一。准确分析合成油中微量残留铁的含量已成为工艺开发过程中至关重要的手段。该文对不同检测方法进行了对比,以燃烧灰化样品等离子体发射光谱检测铁含量的方法对不同沸点的合成油样品进行了验证,并通过实验数据优化了检测方法中的关键步骤。经验证费托合成油样品前处理最优条件为称样量5 g,马弗炉于500℃灰化1 h。该法对铁含量测定的回收率大于95%,相对标准偏差(RSD)不大于5.7%,检出限及定量下限分别为0.15 mg/kg和0.50 mg/kg。     

渤海稠油及其组分中杂原子化合物的负离子电喷雾-高分辨质谱分析

采用沉淀法和色谱分离法将渤海某油田稠油分离成沥青质、胶质、剩余分3个组分。采用负离子电喷雾技术(ESI)结合高分辨傅立叶变换离子回旋共振质谱仪(FT-ICR MS)研究了该稠油及各组分的分子组成。结果表明,剩余分中有较少的极性杂原子化合物能被负离子ESI电离,如N_1,N_1O_1,O_1和O_2类,其等效双键数(DBE)较小。胶质和原油中极性化合物有相同的杂原子类型,包括N_1,N_1O_1,N_1O_2,N_2,N_2O_2S_1,O_1,O_2,其中胶质和原油中N_1,O_1,O_2类化合物的DBE-碳数分布图相似。沥青质中富集高缩合度且多杂原子的酸性化合物,如含杂原子N_,S的氧化程度高的化合物(N_2O_1,N_1O_3,S_1O_3)及O_3类化合物,这些物质具有较高的界面活性,易吸附在界面上促进界面张力降低和增强界面膜强度,从而有利于乳状液稳定存在。N_1O_1,N_1O_2,N_1O_3类化合物,N_2O_1类化合物可能分别是N_1化合物,N_2化合物的氧化降解产物;随着氧化降解程度增加,降解产物的极性明显增强。     

Plant Oil‐Derived Epoxy Polymers toward Sustainable Biobased Thermosets

Epoxy polymers (EPs) derived from soybean oil with varied chemical structures are synthesized. These polymers are then cured with anhydrides to yield soybean‐oil‐derived epoxy thermosets. The curing kinetic, thermal, and mechanical properties are well characterized. Due to the high epoxide functionality per epoxy polymer chain, these thermosets exhibit tensile strength over an order of magnitude higher than a control formulation with epoxidized soybean oil. More importantly, thermosetting materials ranging from soft elastomers to tough thermosets can be obtained simply by using different EPs and/or by controlling feed ratios of EPs to anhydrides.

     

不同等级煤与油共炼的转化率差异及残渣分析

选取安徽褐煤、辽宁褐煤和贵州烟煤三种煤为原料,以油溶性环烷酸钼为催化剂,分别与马瑞常渣(MRAR)、克炼常渣(KAR)以及催化裂化油浆(FCCS)在高压釜内模拟悬浮床加氢共炼反应。结果表明,不同的油体系下,两种褐煤都能达到83%以上的转化率,而对于贵州烟煤,转化率最高的FCCS体系与最低的KAR体系分别为67.75%和50.31%,相差很大。采用FT-IR和SEM分析反应后固体残渣,计算了固体残渣中脂肪族和芳香族中各个基团的相对含量,并对比了不同体系反应后固体残渣的微观形貌。结果表明,KAR体系的固体残渣脂肪链较长,支链化程度高,取代度较低。转化率较高的褐煤反应后固体残渣结构松散,分散度高;转化率较低的烟煤固体残渣随着转化率降低,残渣颗粒逐渐变大,表面更加光滑,板结程度加深。     

多巴胺和L-精氨酸制备超轻氮掺杂石墨烯气凝胶吸油性能的研究

采用水热法制备了超轻氮掺杂石墨烯气凝胶。分析表征结果表明,多巴胺不仅为还原剂而且提供氮源,石墨烯溶液前躯体的pH值对水热法制备超轻氮掺杂石墨烯气凝胶很大的影响,通过调节多巴胺和L-精氨酸在石墨烯溶液前躯体的浓度,可制备密度为2.54 mg/cm³超轻氮掺杂石墨烯气凝胶,由于氮掺杂、低密度和大的比表面积,超轻氮掺杂石墨烯气凝胶对各种油品都有良好的吸附性能。     

胜利断块油藏细分注水技术界限研究

老油田进入特高含水期后,剩余油分布更加零散,各种地质因素也因长期注水开发而发生了一定的改变.此时稳油控水难度进一步加大,为了进一步挖掘剩余油,控制含水上升速度、减缓产量递减,必须对注水井采取进一步的细分调整.基于水湿油藏注水井注水层段吸水效果,从注入水受力分析入手,运用达西定律推导出了水驱油藏水驱油全过程中的单位体积注入水沿竖直、地层两个方向运移的渗流速度公式,明晰了水驱油藏注水层段不同开发阶段砂岩吸水机理.研究结果表明,水驱油藏细分注水效果与岩石绝对渗透率、水相相对渗透率、注入水黏度、水动力压力梯度、注水井启动压力梯度、含水饱和度、地层倾角、油水密度差等参数有关.结合胜利油田断块油藏地质特征及细分注水工艺要求,制定了一套适合胜利油田不同断块区的细分注水技术政策界限:层段内渗透率变异系数小于0.3,砂岩条带宽度极比小于2.5,且东辛油区断块油藏层段内砂岩厚度小于6m,小层数小于4个;现河油区断块油藏层段内砂岩厚度小于5m,小层数小于5个;临盘油区断块油藏层段内砂岩厚度小于6m,小层数小于6个.矿场试验证实,该细分注水技术政策界限是合理、实用的,其为胜利断块油藏注上水、注够水、注好水,实现多层断块油藏的高效开发提供了技术保障,对类似油藏细分注水技术界限研究具有一定的借鉴意义.     

Comparative Study using Raman and Visible Spectroscopy of Cretan Extra Virgin Olive Oil Adulteration with Sunflower Oil

The adulteration of extra virgin olive oil with low-quality and inexpensive seed oil is a serious problem in the industry. In recent years, the characterization of extra virgin olive oil adulteration with various techniques has been successfully implemented. In this work, a comparative study of Raman and visible spectroscopy is presented. These methods are rapid, noninvasive, and no sample pretreatment is required. We used both methods to study Cretan extra virgin olive oil adulterated with sunflower oil. Statistical analysis based on partial least square regression was used to determine the detection limits of the methods. Raman spectroscopy was superior in comparison to visible spectroscopy with adulteration detection limits of 3.5 and 5.5%, respectively, for the same samples. These results indicate that both techniques are suitable for olive oil quality control.     

Dehydration of Castor Oil over NaHSO4/MCM‐41 Catalyst Modified by n‐Dodecyltriethoxysilane

n‐Dodecyltriethoxysilane (DTEOS) modified NaHSO₄/MCM‐41 catalysts (silanized catalysts) were synthesized by different impregnation sequences and evaluated in the liquid‐phase dehydration of castor oil. The samples were evaluated by X‐ray diffraction, nitrogen adsorption‐desorption, SEM, TEM, FT‐IR spectroscopy, XPS, ²⁹Si MAS NMR spectroscopy, contact angle measurements, NH₃‐TPD, and pyridine‐FT‐IR spectroscopy. The analyses demonstrated that silanization enhanced the hydrophobicity of the catalysts, and the impregnation sequence of silanized catalysts had a significant effect on the NaHSO₄ dispersion, surface area, acid distribution, and hydrophobicity of the silanized catalysts. The catalytic activity of the silanized catalysts was much higher than that of NaHSO₄/MCM‐41. Among the silanized catalysts, the catalyst prepared by simultaneous impregnation with DTEOS and NaHSO₄ showed the highest iodine value of 141.8 [g(I₂) per 100 g] and lowest hydroxyl value of 11.3 [mg(KOH) · g^–1].     

Development of a novel hollow‐fiber liquid‐phase microextraction based on oil‐in‐salt and its comparison with conventional one

A novel hollow‐fiber liquid‐phase microextraction based on oil‐in‐salt was proposed and introduced for the simultaneous extraction and enrichment of the main active compounds of hesperidin, honokiol, shikonin, magnolol, emodin, and β,β′‐dimethylacrylshikonin in a formula of Zi‐Cao‐Cheng‐Qi decoction and the single herb, Fructus Aurantii Immaturus , Cortex Magnoliae Officinalis , Radix et Rhizoma , and Lithospermum erythrorhizon , composing the formula prior to their analysis by high‐performance liquid chromatography. The results obtained by the proposed procedure were compared with those obtained by conventional hollow‐fiber liquid‐phase microextraction, and the proposed procedure mechanism was described. In the procedure, a hollow‐fiber segment was first immersed in organic solvent to fill the solvent in the fiber lumen and wall pore, and then the fiber was again immersed into sodium chloride solution to cover a thin salt membrane on the fiber wall pore filling organic solvent. Under the optimum conditions, the enrichment factors of the analytes were 0.6–109.4, linearities were 0.002–12 μg/mL with r ² ≥ 0.9950, detection limits were 0.6–12 ng/mL, respectively. The results showed that oil‐in‐salt hollow‐fiber liquid‐phase microextraction is a simple and effective sample pretreatment procedure and suitable for the simultaneous extraction and concentration of trace‐level active compounds in traditional Chinese medicine.     

蓖麻油基巯烯基紫外光固化胶粘剂的研制与性能研究

以异佛尔酮二异氰酸酯(IPDI)、蓖麻油(CO)、丙烯酸羟丙酯(HPA)为原料,采用熔融缩聚法合成出端丙烯酸酯基预聚体;同时以CO和3-巯基丙酸(3-MPA)为原料采用酯化反应合成出端巯基光引发单体。将端不饱和双键聚氨酯丙烯酸酯预聚体与所制备巯基丙酸酯按一定比例复合,加入光引发剂,在紫外光照射下,预聚体中双键与光引发单体中巯基发生巯基-烯点击反应,制得聚氨酯丙烯酸酯固化膜。采用核磁共振氢谱(1 HNMR)、红外光谱(FT-IR)、热重分析(TG)和光量热系统(Photo-DSC)等手段对合成预聚体、巯基丙酸酯及固化膜结构和性能进行了分析表征。结果表明:在紫外光辐照下,预聚体中不饱和双键与巯基化合物中巯基间发生了自由基加成反应,固化时间在60s以内,且所制备UV固化膜具有良好的机械性能和热稳定性。