Ozone-assisted oxidative desulfurization of light oil fractions

A catalytic system for oxidative desulfurization has been created, which is a transition metal salt bearing an organic ligand and capable of forming an active oxidative complex in the interaction with ozone and further oxidizing sulfur compounds present in fuel followed by the adsorption of the oxidation products on silica gel. In this case, a direct contact of ozone with the fuel is avoided, making the process safer. The effect of the reaction and ozonation conditions on the desulfurization process has been studied. Total sulfur content was decreased to 180 ppm for the straight-run gasoline fraction and to 900 ppm for the diesel fraction.     

原煤测硫仪分析油品硫含量

采用正交实验法,用HXZ－S3测硫仪测定重油、渣油、蜡油中的硫含量,考察了高温炉温度、载气流速、样重等因素对油品中硫回收率的影响,结果表明：在炉温900℃、载气流速1．2L/min、样重为25mg的条件下,硫回收率可达95％以上,且准确度高,重复性好。该法可替代传统的艾士卡重量法用于油品中硫含量的测定。     

测定超低硫柴油产品中硫含量的微库仑分析法

介绍了利用微库仑仪测定超低硫柴油中硫含量的方法。测定的最佳条件是：氧气流量60～80ml／min、流量氩气160mL／min,裂解炉温度900℃,偏压110—150mV,电流20～100μA,进样量3-4μL。测得结果的相对标准偏差均小于5％。实验结果表明,微库仑法具有重复性好、操作简单、结果准确等优点。     

页岩含油率多种测试方法对比

页岩含油率是页岩油资源评价的基本参数,但其测定方法尚无统一认识,制约了页岩油资源潜力的评估准确率。选取松辽盆地页岩油井的密闭取心页岩样品,依次开展二维核磁共振(T₁—T₂ NMR)、有机溶剂蒸馏萃取(Dean Stark)、热解气相色谱(PY-GC)和岩石热解(Rock-Eval)4种页岩含油率测定实验。对比分析表明,T₁—T₂ NMR法与Dean Stark法的页岩含油率测试结果相近,均高于PY-GC法,Rock-Eval法测试结果最低。样品处理方式对页岩含油率的测试结果具有重要影响,块状样品的测试含油率明显高于粉碎样品。综合分析认为,T₁—T₂ NMR法测试页岩含油率结果的可靠性高,具有时间短、样品无损、样品非均质性影响小等特点,是分析页岩含油率的最优手段,具有良好的推广应用前景。建立了不同热演化成熟度页岩的含油率恢复系数、轻烃恢复系数及校正图版,对于湖相I型有机质页岩发育区开展页岩含油率分析具有重要参考价值。     

影响燃料油硫含量分析结果的因素

研究了取样量、灯芯、火焰高度、灯芯管距烟道高度等因素对低硫油品硫含量分析结果可靠性的影响。结果表明,在取样量为(1.8±0.2)g,灯芯疏密及粗细与油品挥发性相适应,灯芯根数随灯芯管内径的增大而增加,火焰高度为6～8mm,灯芯管距烟道6～8mm,燃烧时不冒黑烟、不熄火等最佳操作条件下,采用燃灯法测定低硫汽油的硫含量,可获得准确可靠的测定结果。     

轻质油中总硫含量的测定方法

文中阐述了现用企业标标准Q/SY DH0327-2006<轻质油中总硫含量的测定(紫外荧光法)>在2010年8月修订过程中,考虑1 200 kt/a乙烯工程改扩建完成时,分析仪器设备的相互依托、分析方法的连续性和数据前后对比等原因,同时参考SH/T0689-2000<轻质烃及发动机燃料和其他油品的总硫含量测定法(紫外荧...     

Ultrasound assisted catalytic oxidative desulfurization of diesel oil using CdO nanoparticles

In this paper, sol-gel auto-combustion method is used to synthesize CdO nanoparticles. The synthesised sample is characterized for its size and structure using X-Ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. And some molecular groups containing in the nanoparticle are detected by Fourier transformer Infra Red (FT-IR). Then, the sample is used to remove the organic sulfur from hydrogenation desulfurated diesel under ultrasonic condition. The influence parameters including catalyst dosage, oxidant dosage, oxidation temperature, oxidation time and extracting times are been researched. The obtained result indicates that under the optimal condition, the desulfurization degree can be reached 72.7%.     

单波长色散X射线荧光法在石油产品中硫含量测定中的应用

采用单波长色散X射线荧光光谱仪,建立了测定石油产品中硫含量的分析方法。考察了方法的重复性和准确性,并用该方法测定实际试样中硫的含量。实验结果表明,氯含量标准曲线具有良好的线性,线性相关系数r为0.9996,线性范围0.5 mg/kg~500 mg/kg,实际试样加标回收率为98.33%~100.93%,并将测定结果与ANTEKXI紫外荧光法进行了对比,分析结果基本吻合。本方法适用于石油产品中硫含量的测定。     

单波长色散X射线荧光光谱法测定油品硫含量

利用SINDIE 7039型单波长色散X射线荧光光谱仪,按ASTM D 7039—07标准方法,测定原油、汽油、柴油等油品的硫含量,分析了操作及样品条件对测定结果的影响,考察了方法的准确度和精密度,并将测定结果与仲裁标准SH/T 0689—2000或GB/T 17040—2008进行了对比。结果表明,测试环境、样品组成、薄膜及样品盒等操作条件均会影响测试结果;该方法准确度测定相对标准偏差不超过1.7%,精密度测定90#汽油、0#柴油和原油样品的相对标准偏差均不超过1.4%,柴油加标回收率为93.6%~104.6%,与对应仲裁标准的分析结果基本吻合,能够满足ASTM D 7039—07标准的要求。     

高效液相色谱法测定生物脱硫溶液中单质硫

生物脱硫作为一种新的天然气净化手段,具有净化度高、流程简单、环境污染少、能耗低等特点,在低碳经济发展和环境保护等方面显示出潜在的优势。主要讨论了利用高效液相色谱法测定生物脱硫溶液中的单质硫。用有机溶剂萃取生物脱硫循环液中的单质硫,前处理后在指定高效液相色谱条件下检测单质硫浓度,形成了一套简单可行的测定生物脱硫溶液中单质硫的方法。该方法的检测限为0.04mg/L,加标回收率为103.00%,满足生物脱硫溶液中单质硫的测定需要。同时,讨论了生物脱硫溶液中其余硫副产物对单质硫的干扰。     

Extractive oxidative desulfurization of model oil/crude oil using KSF montmorillonite-supported 12-tungstophosphoric acid

12-Tungstophosphoric acid(PW) supported on KSF montmorillonite, PW/KSF, was used as catalyst for deep oxidative desulfurization(ODS) of mixed thiophenic compounds in model oil and crude oil under mild conditions using hydrogen peroxide(H_2O_2) as an oxidizing agent. A one-factor-at-a-time method was applied for optimizing the parameters such as temperature, reaction time, amount of catalyst, type of extractant and oxidant-tosulfur compounds(S-compounds) molar ratio. The corresponding products can be easily removed from the model oil by using ethanol as the best extractant. The results showed high catalytic activity of PW/KSF in the oxidative removal of dibenzothiophene(DBT) and mixed thiophenic model oil under atmospheric pressure at 75 ℃ in a biphasic system. To investigate the oxidation and adsorption effects of crude oil composition on ODS, the effects of cyclohexene, 1,7-octadiene and o-xylene with different concentrations were studied.     

Peroxide oxidative desulfurization of a mixture of nonhydrotreated vacuum gas oil and diesel fraction

Oxidative desulfurization of a model mixture on the basis of vacuum gas oil and diesel fuel by hydrogen peroxide in the presence of formic acid has been studied. A technology of a two-phase system with a phase-transfer catalyst has been employed for the desulfurization. The optimum reaction time is 6 h and the hydrogen peroxide: sulfur molar ratio is 4: 1. As a result of successive triple oxidative desulfurization, 90% of total sulfur is removed from the model mixture.     

催化裂化柴油氧化萃取脱硫工艺研究

以氧气作氧化剂,甲酸作催化剂,N-甲基吡咯烷酮（NMP）作萃取剂,采用催化氧化反应与溶剂萃取相结合的方法对催化裂化柴油进行了氧化萃取脱硫实验。通过单因素实验考察了催化剂用量,催化氧化温度、时间、氧气压力及萃取剂的用量等对催化裂化柴油硫含量的影响。通过实验得出最适宜的脱硫条件为：反应温度80℃;反应时间90min;充氧压力0．6MPa;催化剂体积分数为10％。经催化氧化,柴油硫质量分数可从1694．2μg/g降到190．8μg/g,脱硫率达到88．7％;在剂油比为1．0和室温条件下,用NMP三级萃取,柴油硫质量分数为37．5μg/g,小于50μg/g,达到欧Ⅳ排放标准的要求。     

高含硫天然气脱硫脱碳工艺技术在普光气田的应用研究

普光气田是我国迄今为止开发的规模最大、丰度最高的特大型海相碳酸盐岩整装气田,天然气中H2S含量高达13%～18%(φ),CO2为8%～10%(φ),有机硫化合物高达340.6mg/m3,常规脱硫脱碳工艺无法适用。该文通过对高含硫工艺技术进行研究分析,制定了普光气田天然气净化工艺路线,选用甲基二乙醇胺(MDEA)作为吸收溶剂,通过催化反应脱除天然气中有机硫,设置级间冷却器控制CO2的吸收,吸收溶剂通过串级吸收、联合再生,降低了装置能耗和运行成本。该工艺在普光气田应用后,外输产品气中H2S含量在6mg/m3以下,CO2含量低于3%(φ),总硫含量低于200mg/m3。     

Modeling of oil generation by Domanik carbonaceous shale

Experiments on artificial maturation of carbonaceous rock of the Domanik age in an autoclave in the presence of water at temperatures of 250, 275, 300 and 325°C have been performed. It has been shown that a significant amount of soluble organic matter (OM) is produced from insoluble OM under these conditions. Changes have been observed in both the biomarker composition of the bitumen and the Rock-Eval OM maturity parameters characteristic of natural catagenesis. By the solid-state ¹³C NMR technique, it has been shown that the amount of aliphatic units decreases and that of aromatic units increases in residual kerogen. Study the product composition of the pyrolysis of residual kerogen has revealed that the relative amount of precursors of n-alkyl structures increases as compared with low-molecular-weight aromatic and thiophenic structures.     

Demetallization and desulfurization of heavy oil residues by adsorbents

The purpose of the work is demetallization and desulfurization of heavy oil residues using adsorbents. Optimal parameters of the demetallization and desulfurization processes of heavy vacuum fraction of Pavlodar Petrochemical Plant LLP in the presence of a zeolite adsorbent containing vanadium oxide xerogel were established: temperature 340?°C, pressure 1?atm., bulk feed rate 1?h^?1. As a result of the process the extraction degree of vanadium, nickel and iron were 90, 70 and 60%, respectively, and the sulfur content decreased from 1.97 to 1.36%. Composition of the chemical adsorbent for demetallization and desulfurization of heavy vacuum fraction is established, too. Content of vanadium, iron and sulfur increase in composition of the adsorbent after treatment of heavy vacuum fraction, which confirms its high adsorption capacity regarding to metals and sulfur.     

基于PSO-BP神经网络的加氢脱硫柴油硫含量的预测研究

针对柴油加氢脱硫生产过程中出现的工艺参数和产品质量难以精准控制的问题,提出粒子群优化(POS-BP)神经网络。基于中国石油大庆石化公司1 300 kt/a柴油加氢脱硫装置生产工艺操作台账数据,选取生产过程中的易波动工艺参数构建训练样本集合和测试样本集合,采用PSO-BP神经网络预测生产操作参数变化时精制柴油产品中硫含量的变化,将POS-BP神经网络与神经网络(BP)和遗传算法优化(GA-BP)神经网络进行横向预测效果比较。实验结果表明,BP神经网络预测的均方误差为2.66×10~(-3),GA-BP神经网络预测的均方误差为2.94×10~(-5),PSO-BP神经网络预测的均方误差为2.41×10~(-5);PSO-BP神经网络预测值与实际值最为接近,且预测结果较佳,具有较好的稳定性和泛化能力,能够精确预测生产操作参数变化时精制柴油产品中硫含量的变化。     

页岩含气量评价方法

作为页岩气资源勘探评价的核心基础,含气量的评价一直作为关键研究内容而受到高度关注.页岩气的成藏和富集是一个动态地质过程,游离和吸附状态天然气的同时存在及比例变化,导致了页岩中天然气赋存状态的复杂性.页岩含气机理与煤层气差异较大,直接和间接成因的页岩气类型各具不同的页岩油气形成条件和含气特点.垂向上的页岩含气相关指征曲线...     

SVDS脱硫技术在硫磺回收装置的工业应用

为了满足GB 31570-2015《石油炼制工业污染物排放标准》的规定,提升区域环境质量,对广泛应用于催化烟气的脱硫技术进行了适应性改造,增加了气-气换热器和高效除雾器等设备,形成适合硫磺回收装置的文丘里脱硫技术(SVDS),并在独山子石化硫磺回收装置进行了工业应用。改造后,排放烟气中SO₂质量浓度从300 mg/m³降至30 mg/m³以下,满足GB 31570-2015中特别排放限值地区SO₂质量浓度的排放要求。在文丘里脱硫技术运行过程中,先后出现气-气换热器压降升高及碱液泵泵壳和叶轮腐蚀的问题,并制定了相应的解决措施,保证了碱洗设施的长周期运行。 