焦化二甲苯中邻二甲苯-间二甲苯分离萃取剂的研究

针对苯加氢过程中产生的二甲苯副产品进行邻间异构体的分离,通过模拟软件Aspen Plus建立的二甲苯分离模型,结合萃取精馏试验对其分离萃取剂进行研究。通过萃取精馏可以实现焦化二甲苯中邻二甲苯和间二甲苯组分的分离;利用二甲基亚砜作为萃取剂时,可以得到95%邻、间二甲苯产品,利用环丁砜作为萃取剂时,可以使间二甲苯产品纯度达到98%,但回收率较低。模拟试验结果为工业生产中实现分离二甲苯异构体提供了必要的基础数据。     

从煤焦油回收洗油中提取联苯的研究

从煤焦油回收洗油中利用减压精馏、二次结晶的工艺路线,先减压精馏去除部分β-甲基萘和α-甲基萘等前馏分,获得纯度为70%左右的富集联苯馏分,进一步结晶去除二甲基萘和吲哚等杂质获得高纯度的联苯产品.研究结果表明在不影响公司物料平衡的基础上可获得99%联苯,并具有较高的产品回收率.该工艺路线,不但回收了宝贵联苯资源,使企业效益最大化,而且使洗苯能力强的有效组分甲基萘等得以浓缩,提高了洗苯洗油的质量,有利于洗苯工序生产.     

2-甲基喹啉的研制

介绍了在实验室用2-甲基喹啉含量70％的原料，加入共沸剂A，采用减压共沸精馏的工艺研制2-甲基喹啉，可得到2-甲基喹啉含量大于95％的产品。     

用气液色谱法测定混合液中苯、甲苯、二甲苯的百分含量

混合液中苯、甲苯、二甲苯的含量一般用精馏方法测定,例如:轻苯组成的分析——苯、甲苯、二甲苯含量的测定是利用试样,经酸碱洗涤脱水后进行精馏,然后分段切取各馏分,而测其含量。但这个方法尚存在着缺点: 1.这个测定需要很长时间,一般四小时以上。     

轻油综合利用技术的应用

传统煤焦油加工工艺最终脱水工序产生一次轻油,焦油蒸馏工序产生二次轻油,两种轻油作为产品销售,轻油潜在价值未得到充分利用。莱钢开发应用轻油精馏提萘及粗苯混配技术,将两种轻油混合回流至馏分塔提取萘,提萘后轻油送至苯加氢系统提取三苯产品,使轻油中的高附加值组分得到综合利用。     

苏联炼焦化学商品(第二部分)

6.两种同分异构的甲酚 C_7H_8O透明油状液体。为间位及对位甲酚之工业混和物,藉分馏由煤提炼的粗酚而得。用以制造塑胶物及染料。产品之比重(d_(20)~(20))应为1.033—1.036,所含间位甲酚(商品的产品计)不小于50％,水份不大于0.8％。开始沸腾不低于195°,最后沸腾(馏出95％)不高于203°。全部溶解于10%烧碱中(允许熔液中有少许之混浊)。在铁路罐车或钢桶运输。2158—49。     

利用铁盐去除钒铬溶液中杂质砷

针对攀枝花红格南矿区钒钛磁铁矿冶炼的钒渣焙烧后浸出液中含砷较高,传统工艺处理时得到的钒产品中砷含量高于国家标准的情况,采用铁盐法除砷,制备高纯的V_2O_5产品。考察了初始p H、温度、反应时间、w_(Fe)/w_(As)、静置沉淀p H等因素对除砷率和钒损的影响。试验结果表明,最佳工艺条件为:初始p H=3,温度40℃,w_(Fe)/w_(As)=4~5,反应时间40~50 min,然后加入Na OH调节p H至6,保温10 min,静置12 h。在此条件下,得到As的去除率大于85%,V的损失率小于5%。溶液中的As含量小于0.08 g/L,得到的V_2O_5(纯度98%)产品中As含量小于0.01%,符合行业标准YB/T 5304-2011。     

大枣多糖铁的合成及其铁含量测定

[目的]从大枣中提取大枣多糖,然后与铁(Ⅲ)合成大枣多糖铁配合物(JPC),建立JPC中铁含量的测定方法.[方法]采用热水浸泡法提取大枣多糖;在碱性条件下,大枣多糖水溶液与三氯化铁反应合成JPC;采用邻菲罗啉分光光度法和原子吸收光谱法测定JPC中铁(Ⅲ)的含量.[结果]JPC是深棕红色无定型粉末,JPC中铁(Ⅲ)的含量:邻菲罗啉分光光度法测定结果为19.76%,原子吸收光谱法测定结果为20.37%.[结论]邻菲罗啉分光光度法和原子吸收光谱法的测定结果基本一致.     

Minitab在炉渣黏度实验数据分析中的应用

利用Minintab软件对高炉渣黏度实验数据进行了单因子方差计算,得到了碱度和化学成分变化对炉渣黏度的影响规律。结果表明:在计算条件下,当炉渣碱度大于1.02,w(MgO)小于11.95%或w(TiO2)小于12.57%时,碱度、MgO和TiO2的含量的变化对炉渣黏度均没有显著影响;而当炉渣碱度小于1.02,w(MgO)大于13.95%或w(TiO2)大于13.57%时,三因素的变化对炉渣黏度有显著影响;炉渣w(Al2O3)控制在12.75%为宜。     

低镉低铁锌的技术改造研究

随着锌用途的扩大,低镉低铁锌出现市场需求。生产中,粗锌通过铅塔、镉塔的精馏精炼得到精锌产品。对铅塔、镉塔进行局部技术改造达到降低成品锌中镉、铁含量的目的,从而满足市场需求。     

Biodegradation of Mixtures of Phenolic Compounds in an Upward-Flow Anaerobic Sludge Blanket Reactor

The anaerobic biodegradability of mixtures of phenolic compounds was studied under continuous and batch systems. Continuous experiments were carried out in up-flow anaerobic sludge bed (UASB) reactors degrading a mixture of phenol and p-cresol as the main carbon and energy sources. The total chemical oxygen demand (COD) removal above 90% was achieved even at organic loading rates as high as 7 kg COD/m3/day. Batch experiments were conducted with mixtures of phenolic compounds (phenol, p-cresol, and o-cresol) to determine the specific biodegradation rates using unadapted and adapted anaerobic granular sludge. Phenol and p-cresol were mineralized by adapted sludge with rates several orders of magnitude higher than unadapted sludge. Additionally, an UASB reactor was operated with the mixture phenol, p-cresol, and o-cresol. After 54 days of operation, 80% of o-cresol (supplied at 132 mg/L) was eliminated. The phenol biodegradation was not affected by the presence of o-cresol. These results demonstrate that major phenolic components in petrochemical effluents can be biodegraded simultaneously during anaerobic treatment.     

氮含量对无镍奥氏体不锈钢力学性能的影响

设计并冶炼了氮质量分数为0.02%～1.20%的无镍奥氏体不锈钢，通过力学性能测试和显微组织观察，研究了氮含量对强度、塑性、韧性的影响。结果表明，氮可显著提高屈服强度和抗拉强度。氮质量分数为0.02%～1.20%时，其与屈服强度和抗拉强度的关系基本为线性关系，并获得了其关系式。韧性对氮含量十分敏感，在氮质量分数为0.39%～0.78%时，冲击吸收功较高，均保持在380 J；氮含量过高或过低时，韧性都会下降。氮含量对断面收缩率的影响较小，氮质量分数在0.78%以下时均超过了70%；而氮质量分数超过0.78%后，塑性则有所下降。当氮质量分数超过0.60%时，拉伸断口上韧窝尺寸随着氮含量的升高而逐渐减小；GN 12N钢断口上出现了大面积的无韧窝区。     

高Ti-Q550钢中Nb、Ti第二相的析出行为

 采用Thermo-Calc软件、热模拟及扫描电镜研究高Ti-Q550钢中微合金的析出规律。采用Thermo-Calc软件计算不同温度下Nb、Ti的析出规律,钛含量对钢中Nb、Ti析出规律及A3的影响。采用热模拟和扫描电镜研究钢中铌相的析出温度。计算结果表明,钛相的析出温度为1498℃,铌相析出温度为1251℃;随着钢中钛含量的增加,(Nb,Ti)C相析出温度和A3温度升高,但铌在钢中的固溶量降低;当钛的质量分数小于0. 08%时,Ti(N,C)相析出温度随钛含量增加而升高,但当钛的质量分数大于0. 08%时,相析出温度基本不变,钛在钢中的固溶量随钛含量增加而增加。     

碳含量对淬火碳钢温变形流变行为的影响

目前关于变形温度、应变速率等因素对流变应力的影响有大量的研究报道,而对温变形条件下碳含量的增加对流变应力的影响规律还缺乏系统研究.基于此开展起始组织为马氏体的不同淬火碳钢温变形流变行为研究.结果表明,在较低温度和较高应变速率(600℃,0.1～1s-1)下,流变应力随碳含量的增加而增大;在较高温度和较低应变速率下(700℃,0.01～0.001 s-1),流变应力在高碳范围内呈下降趋势.碳的质量分数低于0.78％时,淬火碳钢温变形激活能随碳含量的增加而降低;碳的质量分数高于0.78％时,淬火碳钢温变形激活能随碳含量的增加而增加.在相同变形条件下,能量耗散效率最大值随着碳含量的增加呈增大趋势.     

1000MPa级高延伸率Q&P钢的实验室研究

以C-Si-Mn系TRIP钢成分为基础,设计了四种不同Si和Mn含量的合金成分,并采用不同两相区奥氏体化温度的淬火—配分(QP)工艺进行处理,得到了兼具高强度和高塑性的QP钢。其中,当奥氏体化温度为820℃时,0.18C-1.8Si-2.2Mn(质量分数,%)钢和0.18C-1.8Si-2.5Mn钢在抗拉强度达到1 000 MPa以上的同时断后延伸率仍不低于20%,显示了极佳的强塑性结合。利用SEM和XRD等对热处理材料的显微组织进行了表征,结果显示,其显微组织为铁素体、板条马氏体和一定量的残余奥氏体,残余奥氏体多呈块状且被铁素体所包围,且奥氏体化温度为820℃时,材料中的残余奥氏体含量和平均碳浓度均较高。更多且稳定的残余奥氏体在变形过程中发生TRIP效应,可以在不显著降低材料强度的情况下更有效地改善材料的塑性,这也是四种试验用钢经820℃的QP工艺处理后显示出更佳强塑性结合的主要原因。     

高分辨率单道扫描型电感耦合等离子体原子发射光谱法测定高合金钢中铝

在测定基体复杂的高合金钢中铝含量时,采用Al 308.215 nm或Al 394.401 nm作为分析谱线,无需使用复杂前处理方法及干扰因子校正模式,使用高分辨率单道扫描型电感耦合等离子体原子发射光谱仪(ICP-AES)对铬、镍质量分数小于20%,铜、锰、钨、钴质量分数小于5%,钼质量分数小于4%的高合金钢中微量铝进行测定。并与普通分辨率全谱电感耦合等离子体原子发射光谱仪测定高合金钢中铝的方法在光谱干扰方面的情况进行了比对。结果表明:方法中铝的测定下限为0.002%(质量分数);校准曲线采用基体匹配法消除基体效应的影响,线性相关系数达0.999 9以上。按照实验方法测定高合金钢样品中铝含量,结果的相对标准偏差(RSD,n=9)不大于6.2%;标准样品中铝的测定结果与认定值相符。     

锰元素对铜镍合金电化学性能的影响

基于对不同Mn含量的铜镍合金进行3.5 %NaCl(指质量分数,下同)溶液腐蚀实验,测试腐蚀不同时间后的开路电位、电化学阻抗谱和极化曲线。通过分析阻抗谱和极化曲线的变化,建立等效电路模型,利用ZsimpWin软件拟合得出各等效元件的数值,研究Mn元素对铜镍合金电化学性能的影响。结果表明在浸泡初期,Mn含量低(0.53 %)的铜镍合金样品开路电位更正;而在浸泡时间超过7 d后,Mn含量高(1.19 %)的样品开路电位更正。锰含量低的铜镍合金样品生成的腐蚀产物膜较锰含量高的样品更具有保护性,合金中含有低锰含量有助于提高合金的耐蚀性能,降低合金的腐蚀速率.      

电感耦合等离子体原子发射光谱法测定偏钒酸铵中10种杂质元素

样品采用盐酸溶解后,以电感耦合等离子体原子发射光谱法(ICP-AES)同时测定了偏钒酸铵中10种微量杂质元素铝、铁、硅、磷、铅、砷、铬、钾、钠、钙的含量。由于样品溶液中含有2.18 g/L钒和0.78 g/L铵根,故实验重点考察了2.18 g/L钒标准溶液、0.78 g/L铵根标准溶液及两者的混合标准溶液,以及10 mg/L各待测元素标准溶液、水和5%(V/V)盐酸试剂空白的谱线重叠与连续背景叠加等光谱干扰以及基体效应对待测元素测定的干扰影响情况。结果表明:该质量浓度的铵根对测定无影响,部分待测元素灵敏谱线受到钒基较严重的光谱重叠或旁峰干扰;高质量浓度钒的基体效应、连续背景叠加等影响因素导致铝、铁、硅、磷、铅、砷、铬、钙的谱线强度增加,对其产生正干扰,同时高质量浓度钒的基体效应也导致钾、钠的谱线强度降低,对其产生负干扰。为此实验方法采用基体匹配和同步背景校正相结合的校正措施消除了高钒基体影响,同时试验优选了未受光谱干扰的各待测元素分析谱线及其背景校正和检测区域。结果表明,背景等效浓度为－0.000 3%(Na)～0.000 4%(Ca);铝、铁、硅、磷、铅、砷、铬、钙在0.001%～0.60%(质量分数)范围内,钾、钠在0.005%～0.60%(质量分数)范围内,其质量分数与其对应的发射强度呈线性,各元素校准曲线的相关系数均不小于0.999;方法中各元素检出限为0.000 1%～0.000 6%。按照实验方法测定两个偏钒酸铵样品中铝、铁、钾、钠、硅、磷、铅、砷、铬、钙,结果的相对标准偏差(RSD,n=8)分别为小于10%(质量分数为0.001%～0.010%),小于7%(质量分数为0.010%～0.050%),小于3%(质量分数大于0.050%);实验方法用于测定4个偏钒酸铵样品中铝、铁、硅、磷、铅、砷、铬、钾、钠、钙,结果与电感耦合等离子体质谱法(ICP-MS)测定结果相吻合。     

Dose-dependent suppression of toluene metabolism by isopropyl alcohol and methyl ethyl ketone after experimental exposure of rats

In order to examine possible suppression of toluene metabolism due to coexposure to other solvents, female Wistar rats were exposed for 8 h to toluene alone (at 50 or 100 ppm), or in combination with either methyl ethyl ketone (at 50, 100, 200 or 400 ppm) or isopropyl alcohol (at 50, 100, 200, 400, 800 or 1600 ppm). Urine samples were collected for 24 h after initiation of each exposure, and subjected to analysis for two toluene metabolites, hippuric acid and o-cresol, both by HPLC. The excretion of hippuric acid, a major metabolite, was not modified when the concentrations of methyl ethyl ketone or isopropyl alcohol were low, i.e. 100 ppm or below, whereas it was reduced when methyl ethyl ketone or isopropyl alcohol concentrations were twice or more times higher than that of toluene. There were no changes in any cases in excretion of o-cresol, a minor metabolite. The observation after coexposure to methyl ethyl ketone or isopropyl alcohol at low concentration is in line with the negative interaction between toluene and methyl ethyl ketone as well as between toluene and isopropyl alcohol after occupational exposures at low concentrations. Metabolic interaction may take place when the exposure intensity is high, as observed in the present study and also after experimental exposure of volunteers to toluene and m-xylene, or occupational exposure to benzene and toluene.     

Urinary excretion of phenols as an indicator of occupational exposure in the coke-plant industry

OBJECTIVE: In the present study the relationship between the level of exposure to o-cresol and of 2,4- +2,5-, 3,4-, and 3,5-xylenols and the urinary excretion of their metabolites was examined. The mixed exposure to phenolic derivatives of exposed workers during their work shift was monitored by personal air sampling of the breathing-zone air and by measurements of phenol, o-cresol, and xylenol isomer concentrations in shift-end urine. METHODS: The study subjects were 76 men working at a coke plant who were 22-58 years old and 34 nonexposed subjects. Concentrations of phenolic compounds were determined in the breathing-zone air during the work shift, whereas concentrations of phenol, cresol, and xylenol isomers were measured in urine collected after the work shift. Concentrations of phenols in air and urine were determined by gas chromatography with flame-ionization detection. Urine samples were extracted after acid hydrolysis of glucuronides and sulfates by solid-phase extraction. The gas chromatography-mass spectrometry method was applied to identify metabolites in urine samples. RESULTS: The time-weighted average concentrations of phenol, cresol, and xylenol isomers detected in breathing-zone air showed that the exposure level of the workers was relatively low. The geometric mean values were as follows: 0.26 mg/m3 for phenol, 0.09 mg/m3 for o-cresol, 0.13 mg/m3 for p- and m-cresol, and 0.02-0.04 mg/m3 for xylenols at the tar-distillation process. Corresponding urinary concentrations were 10.39, 0.53, and 0.25-0.88 mg/g creatinine for phenol, o-cresol, and xylenol isomers, respectively. The correlation coefficients between the o-cresol and 2,4-, 2,5-, 3,4-, and 3,5-xylenol concentrations measured in urine and in the breathing-zone air were statistically significant, varying in the range of 0.54-0.74 for xylenol isomers and being 0.69 for o-cresol. CONCLUSION: We have found that the presence of o-cresol and xylenol isomers in urine can be used as a biomarker for phenol exposure. Analysis performed on workers at the tar-distillation process showed that they were exposed to relatively low concentrations of phenolic compounds.