润滑油潜含量测定中低毒脱蜡溶剂的选择

针对润滑油潜含量测定方法RIPP9－1990中使用的丙酮-苯-甲苯混合溶剂挥发性大、毒性较高的情况,采用低毒的丁酮-甲苯混合溶剂作为减压蜡油的脱蜡溶剂进行实验研究。根据脱蜡油收率随溶剂组成的变化确定了丁酮-甲苯的适当组成,并且采用不同原油的减压蜡油（VGO）对新、旧两种脱蜡溶剂进行了对比考察。结果表明,由新、旧两种溶剂得到的脱蜡油在性质和质谱组成上基本一致,因而可以用低毒的丁酮-甲苯（体积比60：40）混合脱蜡溶剂替代RIPP9－1990方法中毒性较高的丙酮-苯-甲苯混合脱蜡溶剂。     

Recycling of used motor oil as an alternative method for production feedstock for the conversion processes

Abstract

Used lubricating motor oil is a high pollutant material that requires responsible management. It may cause damage to the environment when dumped into the ground or into water streams including sewers. This may result in groundwater and soil contamination. Recycling of such contaminated materials will be beneficial in reducing lubricating motor oil costs. In addition, it will have a significant positive impact on the environment.

Used oil can be refined to yield base oils that are blended into lubricating products, thus reducing the consumption of virgin oils and it can be used as a feedstock for hydro conversion for production fuels and fuel oil.

This work investigates refining of used lubricating motor oil using solvent extraction method. The laboratory experiment was based on a full factorial design and two categorical factors with two levels were nominated which were solvent to used oil ratio and solvent type (2-Propanol and n-Butanol, MEK and blended the solvents with gazoline).

The type of solvent used and the mixing ratio applied for different runs has shown significant effects on the yield of recovered oil. The yield with bisolvent type MEK+gasoline was higher than the other solvents. The yield of treated oil with butanol mixed with gasoline is 87.5% and it is so close to the yield when we used the butanol alone which is 88.6%.     

废润滑油再生的研究进展

介绍了废润滑油的组成成分;从原理和优缺点两方面综述了硫酸-白土工艺、溶剂萃取、加氢精制等传统再生工艺和分子蒸馏、超临界萃取、膜处理等新型的废润滑油处理工艺;并展望了润滑油再生的前景。随着具有吸附量大、催化效应的纳米材料的快速发展以及稳定性好、耐腐蚀性膜的研究,纳米技术和膜技术将会成处理废润滑油的热点。     

基于三碳醇溶剂精制再生废润滑油

 溶剂精制再生废润滑油具有环保、经济、高效的特点,采用单因素实验方法,以三碳醇(异丙醇、正丙醇)极性溶剂为萃取剂、乙二胺为絮凝剂组合精制再生废润滑油。最佳工艺条件：萃取溶剂异丙醇、精制时间25 min、精制温度40℃、剂/油质量比9、絮凝剂质量分数1.2%。在该精制工艺条件下,再生油的性能指标得到明显改善,黏温指数达130以上、闪点超过210℃、酸值为0.05 mg KOH/g、灰分降至0.01%以下、重金属元素含量显著下降,再生油产率为76.8%,基本上符合HVI150基础油指标,表明该精制工艺再生废润滑油可行,具有广阔的应用前景。     

改善润滑油馏分糠醛精制过程的研究

以糠醛、糠醛与表氯醇混合溶剂分别对大庆油田化工总厂的润滑油馏分进行精制实验。实验的结果表明 ,糠醛与表氯醇混合溶剂的精制过程比糠醛精制过程优越 ,在精制油质量相当的情况下 ,混合溶剂不仅降低了精制温度 ,提高了精制油收率 ,而且降低了精制过程的能耗和剂耗。     

The Reclamation of Fine Lubricating Oil From Flat Lubricating Oil Using a Combination of Activated Animal Charcoal and Amberlite Resin

This study aims at recovering quality rerefined (fine) and metal-free base oil from used lubricating oil. Samples of used lubricating oils were subjected to sedimentation, extraction using methylethylketone and elution using n-hexane on activated animal charcoal, amberlite resin, and ratio 1:1 mixture of activated animal charcoal/amberlite resin separately to produce fine oils. The fine oils obtained, unused, and used (control) lubricating oils of the same brand (Mobil Super XHP SAE 20W-50) were subjected to atomic absorption spectroscopy (Buck Model 205) to determining the levels of 10 wear metals (Fe, Cu, Mn, Cd, Zn, Ni, Cr, Pb, Sb, and Se). Iron has the highest mean concentration (638.56 μg/g), while Mn has the least average level (8.72 μg/g) in the used lubricating oils. Comparison of the elemental concentrations of the rerefined oil with the used and unused (control) lubricating oils indicated that the concentrations of the analyzed wear metals were high in the used and unused (control) lubricating oils. This was corroborated by their t test values. All the three adsorbents used are confirmed to be effective in metal removal from the used lubricating oils, but the mixture (1:1) of the activated animal charcoal/amberlite resin proved to be the best option since the elusion is moderately fast, apart from been an effective metal removal adsorbent, it removed unwanted obnoxious color effectively.     

SOLVENT REFINING OF WASTE LOCOMOTIVE OIL

The potential of ten solvent in the refining of waste locomotive oil have been examined and evaluated The solvents studied were butanone, methyl-isobutyl ketone (MIBK), methyl normal - propyl ketone (MNPK), methyl ethyl ketone (MEK), butyl alcohol, sec-butyl alcohol, pentanol, hexanol, hexane and n-heptane. The solvents were evaluated on the basis of the percent sludge removal, sludge settling rate, oil recovery (yield) and their physico - chemical properties. The optimum settling time and solvent to waste oil ratio were determined to be 24 hours and 5:1 respectively. On the basis of sludge removal potential butyl alcohol ranks first followed by sec-butyl alcohol, butanone, pentanol, hexanol, MEK, MNPK, MIBK, hexane and n-heptane in that order. All the solvents gave very high yields of the refined oils. The physico-chemical properties of the re-refined oils are within acceptable limits. Generally, the properties remained approximately constant regardless of the solvent used for extraction.     

Fabrication of CoNiMo/γ-Al2O3 from waste aluminum foil to convert waste lube oil to hydrotreated oil

Because of the heavy metal content and other toxic chemicals, used lubricating oil remains one of the most serious environmental concerns. The target of this work is the synthesis of γ-Al₂O₃ from waste aluminum foil and re-refining waste lubricating oils using solvent extraction pursued by hydrotreatment. The trimetallic CoNiMo/γ-Al₂O₃ catalyst was prepared via a co-impregnation method. The support and tri-metallic supported alumina are characterized by N₂ adsorption–desorption techniques, X-ray diffraction (XRD), Raman spectroscopy, HRTEM, and EDX. The catalyst was evaluated in the hydrotreating of extracted waste lubricating oils. The results confirmed that the solvent to oil ratio of 3 gave the higher performance with the highest percent of sludge elimination at room temperature. Hydrotreating of extracted lube oil was investigated to determine the effect of variables such as temperature, pressure, liquid hour space velocity, and hydrogen to oil feed ratio. The results indicated that the optimum conditions are (temperature 400 °C, Pressure 60 bar, 0.75 h⁻¹ LHSV). The results showed improvement of the hydrotreated waste lubricating oils properties by decreasing the refractive index from 1.480 to 1.460, the total acid number decreased from 8.164 to 0. 459, the Viscosity Index increase from 78 to 129, and the Sulfur content decreased from 6752 ppm to 543 ppm.     

四碳醇溶剂精制再生废润滑油的研究

针对溶剂精制再生废润滑油环保、经济、高效的特点,应用四碳醇极性溶剂为萃取剂、聚丙烯酰胺为絮凝剂进行再生废润滑油研究,采用单因素实验方法考察工艺条件的影响,得到的最佳工艺条件为：萃取溶剂为异丁醇、精制时间15 min、精制温度25 ℃（室温）、剂油质量比5/1、絮凝剂用量1.0%。该工艺下再生油产率达82.1%,再生油理化指标得到明显改善,黏温指数达130以上、闪点超过200 ℃、酸值为0.01 mg KOH/g、残炭含量降低到0.01%以下,表明采用该精制工艺再生废润滑油是可行的,有广阔的应用前景。     

基于分子管理的渣油掺炼FCC油浆对丙烷脱沥青工艺的影响

以中国石化茂名分公司混炼渣油和催化裂化(FCC)油浆为原料,在渣油丙烷脱沥青小型试验装置上,从分子管理的角度考察FCC油浆掺炼比、溶剂比和抽提温度等操作条件对产物收率及性质的影响。结果表明:掺炼油浆对渣油丙烷脱沥青过程具有协同作用,脱沥青油收率随FCC油浆的掺炼量、溶剂比的增大、抽提温度的降低而提高。在掺炼比30%、溶剂比6、萃取塔上/下段温度60/48℃、压力4.25 MPa的试验条件下,脱沥青油的收率可达31.71%,主要性质如馏分组成、H/C原子比及残炭等符合催化裂化原料的要求;脱油沥青的收率为68.29%,且其针入度、软化点及延度等主要性质符合重交通道路沥青AH-90指标。     

Production of Low Metal Content Re-refined Lubricating Oil

Abstract

A number of metals are found in used lubricating oil. In this article, performance of solvent extraction followed by adsorption on magnesite has been studied for removal of metals from used oil. The suggested process is one of the efficient methods to remove not only sludge, but also the metals either present in the lubricating oil as additives or picked up by the oil during its working life. The re-refined oil has metal content comparable with base oil. In some cases, even lower metal content has been observed.     

再生润滑油着色物质的研究

采用白土精制和溶剂精制工艺对再生润滑油J和B进行了脱色处理,并采用裂解 气相色谱 质谱联用(Py GC/MS)分析方法探究了白土吸附物和萃取物的化学结构。对脱色精制前后的油品进行了氧化安定性评价。结果表明,脱色处理降低了再生润滑油的色度号。J油脱出物中含有较多杂环氮化物或疑似抗氧剂烷基二苯胺氧化产物的含氮化合物,而B油脱出物中氮化物含量较少,但含有多种润滑油使用的添加剂。J油中的着色物质主要是天然氮化物和二烷基苯胺类抗氧剂的氧化产物;B油中的着色物质主要是烃类的氧化产物--酮、醛等衍生物。精制后油品抗氧性能相比于精制前下降比较明显。精制工艺脱出物的分析结果与精制后油品抗氧性能下降的实验现象有一定相关性。     

SUPERCRITICAL FLUID EXTRACTION OF TURKISH LIGNITES AND OIL SHALE WITH TOLUENE MIXTURES

Abstract

Supercritical -Fluid extraction (SFE) of two Turkish lignites and oil shale with toluene mixtures were investigated. Experiments were performed in a batch autoclave at 623 K. Extracts recovered from SFE were fractionated into oils, asphaltenes and preasphal-tenes by solvent extraction.

The conversion of lignites decreased with increasing n-pentane content in the mixture. The extraction yield and the products (oils, AS, PAS) increased with increasing n-pentane content in its range below 15 %

The conversion and the extract yield obtained from Cöynük ail shale is higher with toluene mixture than toluene.     

THE EXTRACTION OF COALS WITH PYRIDINE AND TOLUENE AT 350°C

ABSTRACT

The extraction of three coals with mixtures of toluene and pyridine at 350^°C were compared. The conversion of both the bituminous and sub-bituminous coals Increased as the amount of pyridine in the mixture Increased up to ca 60% pyridine at a constant gas density of 0.64 g/ml. However, there was no Improvement in conversion for the brown coal when toluene was replaced with pyridine. The difference between pyridine and toluene conversion decreased as the gas density decreased. The high solvent efficiency of pyridine is probably due to the unshared pair of electrons on the nitrogen atom. Addition of other compounds with an unshared pair of electrons on a nitrogen or an oxygen atom also Increased conversion In toluene supercritical gas extraction of a bituminous coal at 350^°C and a constant solvent density.     

费-托合成蜡分质分级-萃取精制工艺研究

以内蒙古伊泰费-托合成蜡为原料，采用减压蒸馏与溶剂萃取相结合的工艺技术脱除费-托合成蜡中的异构烃类和含氧化合物以降低其油含量。考察了不同萃取剂、操作条件对脱油效果的影响，采用傅里叶红外光谱（FT-IR）和高温气相色谱对蜡样品进行分析。结果表明：选用N-甲基吡咯烷酮为溶剂，在萃取温度为120 ℃、剂油质量比为2.0:1的操作条件下，萃取得到的精制蜡收率和含油率最佳，分别为93.75%和0.097%，精制蜡滴点为112 ℃，针入度为0.1 mm，产品满足Sasol公司H105费-托合成蜡产品质量标准。精制费-托蜡的碳数分布在C19~C120之间，FT-IR表征结果表明其结构简单，主要由长链正构烷烃组成，C35的含量最高。     

The Improvement of the Quality of Raffinate Obtained from Solvent Extraction of Lubricating Oils

Abstract

Vacuum distillates of an Egyptian crude oil were subjected to solvent extraction process applying N-methyl-2-pyrrolidone (NMP) and furfural as dearomatization solvents. The study shows that the extraction solvent together with the temperature and solvent-to-oil ratio have a significant effect on the yield and quality of produced lubricating oils. The optimum temperature for extracting light waxy distillates with NMP is 55°C at the solvent-to-feed ratio 2:1. These conditions are appropriate to remove the major portion of aromatics from the raffinate. The apparent activation energy (Ea), enthalpy (ΔH*), entropy (ΔS*), and free energy of activation (ΔG*) were calculated for the solvent dearomatization process.     

生产润滑油基础油溶剂精制工艺条件的研究

当今原油价格居高不下,炼好每吨油使工业生产效益最大化,是各石化企业的艰巨任务.文章旨在利用实验室润滑油溶剂精制评价方法,通过溶剂精制和白土补充精制对西江和尼尔(混合比为1∶ 1)减三线、减四线脱蜡油生产HVI基础油进行实验室的最优条件评选,为工业生产和改造提供必要的基础数据.本研究采用间歇模拟法[1]作为润滑油溶剂精制方法,选用油品族组成、油品理化性能等质量数据确定糠醛精制装置理论级数为三级;实验数据也表明用三级逆流萃取实验可以模拟生产中的糠醛精制过程.     

基于分子管理的萃取分离工艺优化利用石脑油资源

In this paper, the separation of aromatics from light naphtha by using extraction process was investigated for improving the utilization efficiency of naphtha. It is indicated that, using a mixture of propylene carbonate-diethylene glycol as the solvent, the optimal extraction conditions cover: a volume fraction of propylene carbonate in the mixed solvent of 0.3, a solvent to feed ratio of 8, and an extraction temperature of 308 K. Through the extraction process, the aromatics mass fraction increases from 10.05% in naphtha to 27.74% in extract oil. It is found that the aromatics yield of extract oil, R_A, reaches 92.11%. As a result, in comparison with naphtha, the potential aromatics content of extract oil increases impressively by 18.03%. Meanwhile, the aromatics content of raffinate oil decreases to 1.33%, and the normal paraffin yield of raffinate oil, Rp, is 76.61%. Accordingly, higher total olefins yields can be obtained when using raffinate oil as the raw material for steam cracking. The present results show that the utilization efficiency of naphtha is improved through extraction process.     

重油沥青质质量分数快速测定方法

采用热溶剂过滤法与抽提回流法（SH/T 0509—2010）,分别以正庚烷和甲苯为萃取剂,对5种重油的甲苯和正庚烷不溶物的元素组成质量分数及形貌进行了分析与表征,并且对比了重油沥青质质量分数的测定数据。结果表明:在萃取剂/原料油（体积/质量比）为30∶1（以甲苯为萃取剂）或100∶1（以正庚烷为萃取剂）,滤膜孔径为0.45 μm,萃取温度为80 ℃的最佳条件下,热溶剂过滤法与抽提回流法所得沥青质质量分数相当。热溶剂过滤法具有分析速度快、适用性强、准确度高的特点,实现了甲苯和正庚烷不溶物质量分数同步测定的目标。     

炼化含油污泥中有机污染物的提取与分析

以中国石化某炼化分公司罐底油泥为原料,考察了甲苯、石油醚、烃类和醇类复配溶剂、石脑油和汽油对含油污泥中有机污染物的萃取效果,选择最优萃取剂进行复配,得到了高萃取率的复合萃取剂,同时考察了剂泥比、萃取温度、萃取时间、搅拌速率对含油污泥有机污染物萃取率的影响,并对提取出的有机污染物和尾砂中的多环芳烃含量进行了测定。结果表明:在复合萃取剂(甲苯/烃类和醇类复配溶剂)质量配比为6∶4、剂泥质量比为3、萃取温度为70℃、萃取时间为30 min、搅拌速率为1 000 r/min的条件下,复合萃取剂对含油污泥中有机污染物的萃取率可达95%以上,萃取量可达0.159 g/mL;提取出的有机污染物中多环芳烃质量分数达到了1 579.87μg/g,其中7种致癌的多环芳烃占44%,潜在的致癌风险较大;尾砂中多环芳烃质量分数小于6μg/g,可直接排放,用作园地、牧草地土壤,不会对环境造成危害。