咪唑酮和咪唑硫酮类羟基衍生物的研究

介绍了杂环化合物咪唑酮和咪唑硫酮类化合物的应用及合成方法。并以4,5-二羟基-1,3-二羟甲基-2-咪唑酮和4,5-二羟基-2-咪唑硫酮为例,介绍了具体的合成步骤及有关数据。     

氨基酸类咪唑啉两性表面活性剂的合成与应用

以二氯乙烷与植物油脂肪酸等为原料,通过氨解、酯化、羟甲基化缩合反应制得氨基酸类咪唑啉型两性表面活性剂。介绍了以它为原料制备产品的用途。     

月桂酸咪唑啉两性表面活性剂的合成及应用

以二甲苯为溶剂 ,月桂酸和二乙烯三氨为原料 ,月桂酸与二乙烯三氨摩尔比为 2∶3 ,在 1 2 0～2 60℃条件下发生酰胺化及环化脱水反应 5～ 6h,再经真空蒸馏脱除过量的二乙烯三氨 ,得浅黄色透明月桂酸咪唑啉产品 ,收率不低于 93 %。将咪唑啉产品与氯乙酸钠溶液反应 ,制得咪唑啉季铵盐两性表面活性剂 ,并对影响该表面活性剂合成的因素进行了讨论。     

兼有缓蚀与降黏性的聚丙烯酸甲酯-丙烯酸咪唑啉制备及性能评价

为开发兼有缓蚀与降黏作用的多功能油品添加剂,以丙烯酸甲酯和丙烯酸咪唑啉为原料制备了聚丙烯酸甲酯-丙烯酸咪唑啉(MA-ACI),用红外光谱对其结构进行了表征,用凝胶渗透色谱对其分子量进行了检测。采用旋转挂片和电化学Tafel极化曲线法评价了MA-ACI的缓蚀性能,用旋转黏度计研究了MA-ACI的降黏性能。结果表明,在丙烯酸甲酯与丙烯酸咪唑啉摩尔比8∶1、引发剂偶氮二异丁腈加量1.0%、反应温度80℃、反应时间10 h的条件下制得的MA-ACI(相对分子质量36582)对N80金属钢片具有良好的缓蚀作用,对江苏油田韦5-57井原油具有较好的降黏作用。在30℃、MA-ACI加量为0.10 g/L时,用旋转挂片法测得的缓蚀率为82.06%,MA-ACI加量为0.40 g/L时,用电化学极化曲线法测得的缓蚀率为90.21%;在70℃、MA-ACI加量为100μg/g时,江苏油田韦5-57井原油的降黏率为85.28%。     

1-对甲硫基苯基-2-甲基-2-吗啉基-1-丙酮的合成与应用

以α溴代酮和甲醇钠为原料 ,甲醇为溶剂合成了中间产物 1甲氧基 1对甲硫基苯基 2 ,2二甲基环氧乙烷 ;回流状态下 ,使该中间产物与吗啉反应 ,合成了题述产物 ,纯度 99.6% ,总收率 84 .6%。并用其制UV固化涂料时 ,在空气和绝氧条件下 ,固化速度优于安息香二甲醚。     

饱和CO2盐水中咪唑啉分子结构与其缓蚀性能的关系

用极化曲线法和静态挂片法评价了不同疏水链和亲水基的系列咪唑啉在饱和CO2盐水中的缓蚀性能,探讨了咪唑啉分子结构与其缓蚀性能的关系。实验结果表明,对于NaC l质量浓度低于50 g/L的饱和CO2的腐蚀介质,咪唑啉的疏水链越长,缓蚀性能越好,若疏水链含有双键则可以进一步提高缓蚀性能;增加腐蚀介质中NaC l的质量浓度,导致疏水链较长的1-氨乙基-2-十五烷基咪唑啉乙酸盐、1-氨乙基-2-十七烷基咪唑啉乙酸盐和1-氨乙基-2-十七烯基咪唑啉乙酸盐的缓蚀性能降低,而疏水链较短的1-氨乙基-2-十一烷基咪唑啉乙酸盐和1-氨乙基-2-十三烷基咪唑啉乙酸盐的缓蚀性能略有升高,但仍以1-氨乙基-2-十七烯基咪唑啉乙酸盐的缓蚀性能最好。在以氯乙酸、醋酸和氨基磺酸对十七烯基咪唑啉改性形成的4种缓蚀剂中,1-氨乙基-1-羧甲基-2-十七烯基氯化咪唑啉的缓蚀性能最好,而氨乙基咪唑啉的缓蚀性能则优于羟乙基咪唑啉。     

饱和CO2盐水中咪唑啉分子结构与其缓蚀性能的关系

用极化曲线法和静态挂片法评价了不同疏水链和亲水基的系列咪唑啉在饱和CO2盐水中的缓蚀性能,探讨了咪唑啉分子结构与其缓蚀性能的关系.实验结果表明,对于NaCl质量浓度低于50 g/L的饱和CO2的腐蚀介质,咪唑啉的疏水链越长,缓蚀性能越好,若疏水链含有双键则可以进一步提高缓蚀性能;增加腐蚀介质中NaCl的质量浓度,导致疏水链较长的1-氨乙基-2-十五烷基咪唑啉乙酸盐、1-氨乙基-2-十七烷基咪唑啉乙酸盐和1-氨乙基-2-十七烯基咪唑啉乙酸盐的缓蚀性能降低,而疏水链较短的1-氨乙基-2-十一烷基咪唑啉乙酸盐和1-氨乙基-2-十三烷基咪唑啉乙酸盐的缓蚀性能略有升高,但仍以1-氨乙基-2-十七烯基咪唑啉乙酸盐的缓蚀性能最好.在以氯乙酸、醋酸和氨基磺酸对十七烯基咪唑啉改性形成的4种缓蚀剂中,1-氨乙基-1-羧甲基-2-十七烯基氯化咪唑啉的缓蚀性能最好,而氨乙基咪唑啉的缓蚀性能则优于羟乙基咪唑啉.     

油溶性咪唑啉的合成及对CO2的缓蚀性能

模拟庆深气田CO2分压范围和采出水矿化度配制腐蚀介质,以异丁醇为溶剂、乳化剂等配制含羟乙基咪唑啉的缓蚀剂,参照《油田采出水缓蚀剂性能评价方法（SY/T 5237—2000）》,测定合成物和复配体系对N80钢试片的缓蚀率。单独使用咪唑啉缓蚀剂的缓蚀效果不理想,缓蚀性能受温度和CO2分压影响较大。将咪唑啉缓蚀剂与适量硫脲、乙二胺在正丁醇、乳化剂、水中进行复配,缓蚀性能有了很大的改善,加药量为500 mg/L的情况下,缓蚀率可达94.65%。     

水溶性咪唑啉酰胺的合成及其缓蚀性能

以壬酸、冰乙酸和多乙烯多胺为原料,在甲苯回流条件下反应合成脂肪酰胺中间体,再升温闭环合成水溶性咪唑啉酰胺。采用红外光谱对产物进行分析表征,考察不同质量分数和不同温度下咪唑啉酰胺水溶液的稳定性。利用铁离子质量浓度法对其在HCl-H_2S酸性溶液中对低碳钢(A_3)的缓蚀性能进行了研究。结果表明,咪唑啉酰胺是水溶性良好的化合物,在HCl-H_2S体系中缓蚀性能优异,其缓蚀率随咪唑啉酰胺质量浓度的增加而增大,当质量浓度为15 mg/L时,其缓蚀率可达80%以上。     

La3+、Pr3+、Nd3+、Eu3+-β-二酮-邻菲绕啉衍生物三元螯合物的合成与表征

以1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮(PMBP)为第一配体,5-丙烯酰胺基-1,10-邻菲绕啉为第二配体,分别合成了铈组稀土元素(La3+、Pr3-、Nd3-、Eu3+)的三元螯合物。用UV、IR、1HNMR、Ms等手段确证了该4种铈组稀土金属-β-二酮-邻菲绕啉衍生物三元螯合物的结构为Ln-(PMBP)3-(5-丙烯酰胺基-1,10-邻菲绕啉)。     

Separation of Paraffin Wax Using Solvent Fractionation

In order to separate and characterize some grades of paraffin waxes from El-Ameria crude waxes (slack waxes), a one-stage fractional crystallization technique has been done to separate the paraffin waxes with different characteristics by using different solvents and solvent mixtures at ambient temperature of 20°C and fixed dilution and washing solvent ratios (S/F) of 4:1 and 2:1 by weight, respectively. The fractionating solvents used are n-hexane, methyl isobutyl ketone (MIBK), dioxane, ethyl acetate, and butyl acetate as a single solvent and a mixture of methyl ethyl ketone (MEK) containing benzene (B) and toluene (T) as a mixed solvent. The resulting data revealed that dioxane and n-hexane solvents are not suitable for fractional crystallization of slack waxes, and the most suitable solvents for separating paraffin waxes with the standard specifications are ethyl and butyl acetates, MIBK, and the mixture of MEK, B, and T (60:20:20 by weight, respectively).     

Separation of Paraffin Wax Using Solvent Fractionation

Abstract

In order to separate and characterize some grades of paraffin waxes from El-Ameria crude waxes (slack waxes), a one-stage fractional crystallization technique has been done to separate the paraffin waxes with different characteristics by using different solvents and solvent mixtures at ambient temperature of 20°C and fixed dilution and washing solvent ratios (S/F) of 4:1 and 2:1 by weight, respectively. The fractionating solvents used are n-hexane, methyl isobutyl ketone (MIBK), dioxane, ethyl acetate, and butyl acetate as a single solvent and a mixture of methyl ethyl ketone (MEK) containing benzene (B) and toluene (T) as a mixed solvent. The resulting data revealed that dioxane and n-hexane solvents are not suitable for fractional crystallization of slack waxes, and the most suitable solvents for separating paraffin waxes with the standard specifications are ethyl and butyl acetates, MIBK, and the mixture of MEK, B, and T (60:20:20 by weight, respectively).     

Tetrathioadamantanes as lubricating oil additives

Summary The following compounds have been synthesized and tested as antiseize and antiwear additives: 1,3,5,7-tetra-methyl-2,4,6,8-tetrathioadamantane; 1,3-dimethyl-5,7-diethyl-2,4,6,8-tetrathioadamantane; 1,3-dimethyl-5,7-dusobutyl-2,4,6,8-tetrathioadamantane; 1,3,5,7-tetramethyl-2,4-dioxo-6,8-dithioadamantane.It has been established that tetrathioadamantane derivatives can serve as additives for mineral oils at elevated temperatures and with p_c up to 140 kg.Translated from Khimiya i Tekhnologiya Topliv i Masel, No. 12, pp. 41–44, December, 1965     

稀土改性复合固体超强酸SO_4~(2-)/TiO_2-MoO_3-La_2O_3催化剂催化合成缩醛(酮)

研究了稀土改性复合固体超强酸SO42-/T iO2-M oO3-La2O3催化剂的制备方法,催化剂的适宜制备条件为:n(La3+)∶n(T i4+)=1∶34、M oO3的质量分数25%、硫酸的浸泡浓度0.5mol/L、硫酸浸泡时间24h、焙烧温度450℃、活化时间3h。以SO42-/T iO2-M oO3-La2O3为催化剂,对以乙酰乙酸乙酯、环己酮、丁酮、苯甲醛、正丁醛与二元醇(乙二醇、1,2-丙二醇)为原料合成10种缩醛(酮)的反应条件进行了研究,较系统地研究了醛(酮)与二元醇摩尔比、催化剂用量、反应时间对收率的影响。实验结果表明,在n(醛(酮))∶n(乙二醇(1,2-丙二醇))=1.0∶1.5、催化剂用量占反应物料总质量的0.8%、环己烷为带水剂、反应时间60m in的条件下,10种缩醛(酮)的收率在56.9%~88.2%之间。     

Friedel-Crafts Acylation of Aromatic Compounds in Ionic Liquids

Abstract

This article first reviews the application of ionic liquids in Friedel-Crafts acylation reactions. Ionic liquids can be used as catalyst solvents, the active component on solid carriers, or just as the solvent. One advantage of using ionic liquids in acylation reactions is the enhanced reaction rates, conversion, and selectivity. The acylation mechanisms of aromatic compounds in ionic liquids are also reviewed and analyzed. The acetylium cation [RCO]⁺ was confirmed to be the key intermediate in the acetylation reactions, and the replacement of a traditional solvent with the ionic liquid did not alter the acylation mechanism. With good consideration, we propose two rational acylation mechanisms for the Friedel-Crafts acylation of aromatics in the Lewis acidic ionic liquid and in the Lewis acid-ionic liquid system. Although the reaction rates, the conversion, and the selectivity for the acylation in ionic liquids are high, the separation of aryl ketone products from ionic liquids and the recycle of the ionic liquids are still a problem.     

复合溶剂间歇萃取精馏分离乙酸乙酯-乙醇物系

使用单一溶剂N,N-二甲基甲酰胺(DMF),二甲基亚砜(DMSO)和复合溶剂DMF-DMSO对乙酸乙酯-乙醇物系进行了间歇萃取精馏的实验。考察了溶剂种类、溶剂比、回流比等因素对分离效果的影响,比较了使用单一溶剂和复合溶剂时的间歇萃取精馏实验所需的操作时间。实验结果表明,复合溶剂DMF-DMSO的分离效果最好,采用复合溶剂DMF-DMSO时,适宜操作条件:n(DMF):n(DMSO)=2:3,溶剂加入速率25mL/min,溶剂与产品质量比5.0,回流比3.3,此时塔顶产品中乙酸乙酯的质量分数为99.52%;且使用复合溶剂DMF-DMSO时间歇萃取精馏的操作时间比使用单一溶剂所需的操作时间短,单位质量产品能耗较使用单一溶剂DMF时降低了42.6%,较使用单一溶剂DMSO时降低了37.4%。     

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.     

高效液相色谱法分析车用料挥发性醛酮类化合物

使用2,4-二硝基苯肼(DNPH)采样管,建立了一种高效液相色谱(HPLC)法分析车用料挥发性醛酮类化合物的方法。结果表明:经优化得到分离度最佳的HPLC分析条件为:选用Analytical C 18型色谱柱为分离柱,以乙腈和水为流动相,V(乙腈)/V(水)为70/30,柱温为45℃,流速为1.0 mL/min,进样量为25μL;一次进样能够使13种挥发性醛酮类物质有效分离,完成1个试样的检测时长约为25 min;对于中国石油兰州石化公司的车用料SP 179,在所得最佳HPLC分析条件下,13种醛酮类化合物的质量浓度在0.045~3.000 mg/L内各组分标准曲线的相关系数均等于1,具有良好的线性关系,且各组分的分离度均大于1.1;而且,当在DNPH管添加3个不同质量浓度为0.03,0.06,0.09 mg/L的13种醛酮的混合标准溶液标样后,车用料SP 179中的DNPH采样加标回收率为96.67%~104.44%,3次重复加标回收测定结果的相对标准偏差为0.92%~6.90%。该方法快捷、准确可靠,可适用于车用料中挥发性醛酮类化合物的检测分析。     

β-二酮镍-烷基铝催化丙烯线性齐聚反应的研究

研究了用 Ni(acac)_2(2,4-戊二酮镍)或 Ni(dPP)_2(1,3-二苯基-1,3-丙二酮镍)/烷基铝均(?)催化体系进行的丙烯齐聚反应。用一系列 Et_2AIY 型的烷基铝(Y=((?)-C_6H_(12))_2N—、C_2H_5O—、n-C_4H_9O—、n-C_(?)H_(11)CO_2—、C_6H_5CO_2—等)作助催化剂时,发现催化剂活性与 Y 的电负性有关,而且只有当 HY 的酸性与β-二酮配体的酸性相适应时,催化剂才有离活性。     

润滑油糠醛精制-催化裂化回炼油抽提组合工艺(Ⅲ)

主要介绍以分离出析出油后的减二线抽出液为溶剂的芳烃抽提小试实验，并与以纯糠醛、润滑油糠醛精减二线抽出液为溶剂的抽提效果进行了对比。结果表明：在相同的抽提条件，以抽出液为溶剂，其抽余油及抽出油收率明显高于以纯糠醛为溶剂所得的收率，其抽余油质量在3种溶剂抽提方式中最差；以分出油后的抽出液为溶剂的抽提效果居中。尽管以抽出液为溶剂时，其抽提效果不如纯糠醛的好，但可以通过调整操作条件来保证抽余油的质量及抽出油的质量。以抽出液为溶剂，其抽出油及抽余油收率均很高，且采用抽出液溶剂时，其溶剂回收系统可与润滑油糠醛精制共用一套，由此可使设备投资及操作费用大大降低。