异丙醇一步法生产甲基异丁基酮分离过程的研究

对异丙醇一步法合成甲基异丁基酮工艺的分离过程进行了基础测定,包括气液平衡和液液平衡测定;对原有的甲基异丁基酮分离工艺进行了研究,应用萃取精馏的原理,提出了改进的工艺流程设想,预计可使甲基异丁基酮的回收率由32％提高到91．7％,每吨产品消耗蒸气由11．42t降至8．27t。     

硼酸三甲酯-甲醇-氯化锂体系液液平衡的测定

分别采用Othmer法和液液平衡釜法测定了298.15K下硼酸三甲酯-甲醇-氯化锂三元体系的液液平衡数据。实验发现：氯化锂的摩尔分率对硼酸三甲酯在甲醇中的溶解度影响较大。在平衡的酯相和醇相中,当醇相中氯化锂的质量百分数小于12．99％时,醇相的密度小于酯相;当醇相中氯化锂的质量百分数大于14．24％时,醇相的密度大于酯相;酯相中硼酸三甲酯的质量百分数最高达98.8％,而氯化锂仅为0．01％。液液平衡的测定为氯化锂盐析工艺提供基础研究。     

正丙醇—水—乙酸钾体系汽液平衡数据的测定及关联

正丙醇－水－乙酸钾体系汽液平衡数据的测定及关联武文良张雅明王延儒时钧（南京化工大学化学工程系，南京２１０００９）关键词正丙醇乙酸钾汽液平衡１引言正丙醇是重要的化工原料和有机溶剂，在常压下与水形成恒沸物（含水５６．８３ｍｏｌ％），用普通方法难以分离。...     

含辛烯醛体系的液液、汽液相平衡研究

测定了水-辛烯醛、水-正丁醇二元系在常压下的液液平衡数据及26.66kPa下的正丁醇-辛烯醛二元系和水-正丁醇-辛烯醛三元系的汽液平衡数据.由测定的3对二元数据求取了NRTL常数及有规参数,并与三元数据进行拟合,计算值与实验值符台良好,液液平衡与汽液平衡得到了统一的关联.     

异丙醇一步法生产甲基异丁基酮分离过程的研究

随着我国经济的发展．涂料对高档溶剂甲基异丁基酮(MIBK)的需求将迅速增加，因此，MIBK的市场市景非常广阔。预计到2005年，我国MIBK消费量为3万t．年均增长率为11％。     

低浓度下己内酰胺-水-硫酸铵-苯体系的液液平衡问题

介绍了在己内酰胺废水中萃取回收己内酰胺的过程中，测定了4套己内酰胺—水—硫酸铵—苯体系的液液平衡数据(水相己内酰胺质量分数小于13％)。实验结果表明，用苯从废水中萃取回收己内酰胺时，pH在2～5．7范围内，pH值升高对回收有利。同时提出了一个简单的关联式并成功地关联上述平衡数据，已用于萃取塔的设计计算。     

加盐萃取精馏分离环己烷-四氢呋喃的研究

进行了环己烷-四氢呋喃物系的加盐萃取精馏实验研究。将NaSCN、NANO3、KI三种盐溶于N,N-二甲基甲酰胺中进行加盐汽液平衡实验,实验表明NaSCN能最大限度地提高体系的相对挥发度．NaSCN的适宜质量分数为8％-13％;进行了间歇加盐萃取精馏分离环己烷-四氢呋喃的工艺研究．结果表明NaSCN质量分数为13％,溶剂比为1：1,溶剂流率为10mL／min为适宜的实验操作条件。     

Study on hybrid pervaporation/distiilation process for methyl-isobutyl-ketone synthetic liquid separation

对丙酮一步法生产甲基异丁基酮(MIBK)部分精馏流程进行了工艺分析,MIBK脱轻塔进料液中少量水的存在使MIBK脱轻塔运行不稳定,进而影响MIBK合成液的整个分离过程.针对这个问题,提出了精馏-渗透汽化集成的工艺方案,省去MIBK脱轻塔.建立了渗透汽化小试实验,研究了NaA分子筛膜的渗透汽化过程以及分离性能.用Aspen Plus软件对精馏-渗透汽化集成工艺进行了模拟,与精馏过程相比,在MIBK产品质量与收率相同情况下,操作成本降低了20％,总成本可降低15％.     

卧式沉降离心机分离沉淀硫酸钡的研究

阐述了硫酸钡生产过程中固液分离工艺的现状。提出了用卧式沉降离心机来代替该行业常用的真空叶滤机或箱式压滤机来分离沉淀硫酸钡，并优化卧式沉降离心机的工艺参数：转速3000r／min，溢流直径138mm．差转速30r／min。在该条件下，经过卧式沉降离心机分离后的硫化钠水溶液质量分数为4．46％～5．30％，硫酸钡钡饼含硫化钠碱液质量分数22％～25％，碱回收率大于95％。该设备用于沉淀硫酸钡生产中固液分离，完全能够满足工艺要求。     

醇-水-醋酸钠/碘化钾体系汽液平衡

用改进的Othmer汽液平衡釜测定了101．3kPa下盐摩尔分率x3=0.008、0.012、0．02乙醇—水—醋酸钠／碘化钾体系；x3=0.01异丙醇／正丙醇—水—醋酸钠／碘化钾体系，共10组汽液平衡数据，并用Mock模型、Sander模型、Macdo模型和Kikic模型对这10组实验数据分别进行了关联，结果良好，基本上满足工程设计要求。其中，Mock模型明显好于其他三类模型，所需模型参数也较少，Sander模型与Macedo模型精度相仿，但Macedo模型消除了D-H项中的不一致性。     

异丙醇一步法合成MIBK精馏过程优化

用PROII过程模拟软件对异丙醇一步法合成甲基异丁基酮(MIBK)的精馏系统进行了分析和模拟优化,提出了5塔流程的改进工艺,使MIBK的回收率提高了2.8倍,达到91·7%,而且再沸器能耗由12·79t水蒸气/t产品降低到8·27t水蒸气/t产品。还建立了普通精馏塔和萃取精馏塔小试实验装置,对全工艺流程逐塔进行热态研究,验证了其工业可行性。     

Improvement of separation process of synthesizing MIBK by the isopropanol one-step method

The separation process of synthesizing MIBK (methyl isobutyl ketone) by an isopropanol one-step method, in which the multi-component mixture contains AC (acetone), IPA (isopropanol), water, MIBK, MIBC (methyl isobutyl carbinol), DIBK (di-isobutyl ketone), etc., was studied. As a high-purity of MIBK over 99.5 wt% is required in industry, the development of an effective separation method is urgent. In this work, first, by means of VLE (vapor-liquid equilibrium) experiments and PROII simulation, the possible azeotropes formed in the investigated system were tested. Then, the separation process was simulated with the result that the calculated and designed values were in good agreement, which indicated that the calculated results were reliable. On this basis, the original separation process was improved. In the original separation process, the yield of MIBK for a concentration of MIBK over 99.5 wt% was small, only 32.5%. In the improved separation process (step two), two columns (one extractive distillation column and the other solvent recovery column) were added and some simplification was made so as to recycle MIBK. In this case the yield of MIBK was 91.7%. Moreover, about 27.6% water stream per kilogram MIBK product is saved.     

基于ASPEN软件对比两种萃取剂在煤气化废水酚回收中的应用

针对某煤气化厂酚回收工艺流程净化废水中酚含量未达到生化处理要求的问题,分析认为主要是由于原萃取剂二异丙基醚(DIPE)对酚分配系数过低。然后以对酚的分配系数更高的甲基异丁基酮(MIBK)为萃取剂,重新设计工艺流程并确定新流程的工艺参数同时对其进行模拟计算,结果显示,净化废水酚含量降至362mg/L,能够满足后续生化段要求;与原流程相比,新流程的粗酚回收量约多0.96 t/d。新旧流程经济核算表明,采用MIBK为萃取剂的流程处理每吨水的价格比DIPE为萃取剂低1.6元。     

甲基异丁基酮分离过程中精馏-渗透汽化集成工艺的研究

对丙酮一步法生产甲基异丁基酮(MIBK)部分精馏流程进行了工艺分析,MIBK脱轻塔进料液中少量水的存在使MI-BK脱轻塔运行不稳定,进而影响MIBK合成液的整个分离过程。针对这个问题,提出了精馏-渗透汽化集成的工艺方案,省去MIBK脱轻塔。建立了渗透汽化小试实验,研究了NaA分子筛膜的渗透汽化过程以及分离性能。用Aspen Plus软件对精馏-渗透汽化集成工艺进行了模拟,与精馏过程相比,在MIBK产品质量与收率相同情况下,操作成本降低了20%,总成本可降低15%。     

丙酮一步法生产MIBK装置的副产物精馏分离研究

针对丙酮一步法生产MIBK装置的副产物（丙酮、异丙醇、水、MIBK混合物）,采用间歇精馏分离得到纯度〉98％的丙酮、纯度〉99％的异丙醇和水恒沸物、纯度〉90％的MIBK。对分离得到的纯度〉99％的异丙醇和水恒沸物用乙二醇作为萃取剂进行萃取精馏分离得到纯度99．5％异丙醇,同时减压精馏回收乙二醇。     

以纳米二氧化锆为载体的Pd催化剂制备及还原缩合性能研究

考察了不同制备方法得到的纳米二氧化锆为载体担载Pd催化剂对丙酮还原缩合的影响。纳米二氧化锆的制备方法对二氧化锆的物理性质和催化性能有较大的影响。不同的沉淀方法、陈化环境制备的纳米ZrO2,对不同的产物有不同的选择性,其中,在母液中373K陈化的二氧化锆为载体的催化剂对二异丁基酮(DIBK)的选择性较高,为61 43%;沉淀剂滴加到盐溶液中得到的二氧化锆为载体的催化剂对甲基异丁基酮(MIBK)的选择性较高,为63 70%。催化剂的酸性和Pd分散度表征结果表明,较高的Pd分散度、合适的酸性有利于MIBK的生成,较高的Pd分散度、较强的酸性有利于DIBK的生成。     

One-step synthesis of methyl isobutyl ketone from acetone and hydrogen over Pd/(Nb2O5/SiO2) catalysts

The surface-phase oxides of niobia on silica substrate ((Nb₂O₅/SiO₂), NS(x)) were prepared and characterized. Such oxides were used as supports for palladium catalysts. The one-step synthesis of methyl isobutyl ketone (MIBK) from acetone and hydrogen in liquid phase was also investigated over Pd/NS(x) catalysts. Experimental results indicate that these catalysts were effective for the formation of MIBK; since little of the parallel by-product of isopropanol (IPA) was formed, these catalysts reached selectivities of 88–92% MIBK and 2–3% IPA at 30–35% conversion. The reactivity of Pd/NS(x) declined obviously with an increase of water content that accumulated in a semi-batch reaction system. The water could be partially expelled and the deactivation of catalysts could be improved by using a fixed bed continuous flow reaction system.     

Selective Extraction of Mercury(II) by 1‐Naphthylthiourea–Methyl Isobutyl Ketone System

Abstract

Selective extraction of Mercury(II) using 1‐naphthylthiourea–methyl isobutyl ketone (ANTU‐MIBK) system from hydrochloric acid solutions (0.1–10 M) has been studied. Influence of foreign ions, acid and ligand concentrations has been investigated. Addition of ANTU in MIBK enhanced, extraction capacity of MIBK to several times. Low effect of foreign ions and high separation factors for a number of metal ions determined at 0.5 M hydrochloric acid concentration evaluated the proposed method efficient and selective. The experimental data obtained from application of the method for extraction of mercury from a synthetic aqueous solution reveal that more than 99% mercury can be separated from cadmium, zinc and selenium in a single step with five minutes equilibration.     

TBP, MIBK/FeCl3与Li形成萃合物组成的研究（英文）

To study the characteristic of liquid-liquid extraction equilibrium of lithium from brine sources,the complexes formed from tributyl phosphate(TBP) and methyl isobutyl ketone(MIBK) with lithium were investi-gated using FeCl3 as coextracting agent.Liquid-liquid extraction reaction mechanisms were proposed and the stoichiometry of tetrachloroferrate(III) complex with lithium was obtained by regressing the experimental data.It is found that the stoichiometry of tetrachloroferrate(III) to lithium in the complex is 1︰1 with either TBP or MIBK as extractant in kerosene.The stoichiometry of the complex of TBP with Li was 1︰1 and that of MIBK with Li was 2︰1.The formed complexes of TBP and MIBK with lithium are determined to be LiFeCl4?TBP and LiFeCl4?2MIBK,respectively,according to the rule of neutralization.