Separation process of butanol-butyl acetate-methyl isobutyl ketone system by the analysis to residual curve and the double effect pressure-swing distillation

The separation of ternary mixture of butanol,butyl acetate,and methyl isobutyl ketone (MIBK) was initially analyzed by the residual curve.In this process,MIBK was chosen as the azeotropic agent during the first step of separation.The optimum mass ratio of extra MIBK was 1.6 in the modified feed stream according to the residual curve.Thus on this condition the top product was butanol-MIBK azeotrope while the bottom product was butyl acetate in the preliminary separation of the mixture.Then the butanol and MIBK azeotrope was separated by the double effect pressureswing distillation with the low pressure column performing at 30 kPa and the atmosphetic pressure column at 101 kPa.The optimal operating conditions were then obtained by using Aspen Plus to simulate and optimize the process.The results showed that the mass purities of butanol,butyl acetate,and MIBK were all more than 99％ and reached the design requirements.Additionally,compared with the traditional distillation with outside heating,the double effect pressure swing distillation saved the reboiler duty by 48.6％ and the condenser duty by 44.6％.     

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.     

Influence of the metal function in the “one-pot” synthesis of 4-methyl-2-pentanone (methyl isobutyl ketone) from acetone over palladium supported on Mg(Al)O mixed oxides catalysts

Pd/Mg(Al)O samples (0.05 < Pd < 0.5 wt%) were evaluated in the gas phase reaction of acetone with hydrogen to methyl isobutyl ketone (MIBK). The catalysts were prepared by impregnating a calcined Mg–Al layered double hydroxide with Pd acetylacetonate in toluene solution. The highest selectivity to MIBK was achieved with ca. 0.2 wt% Pd and size of Pd particles of ca. 3–5 nm.     

甲基异丁基酮的生产方法及其应用

介绍了甲基异丁基酮（ＭＩＢＫ）国内外现状、生产方法和用途。重点介绍了丙酮法。建议国内采用丙酮常压一步法工艺习快建立ＭＩＢＫ生产装置,以满足ＭＩＢＫ不断增长的需要。     

SML resist processing for high-aspect-ratio and high-sensitivity electron beam lithography

A detailed process characterization of SML electron beam resist for high-aspect-ratio nanopatterning at high sensitivity is presented. SML contrast curves were generated for methyl isobutyl ketone (MIBK), MIBK/isopropyl alcohol (IPA) (1:3), IPA/water (7:3), n-amyl acetate, xylene, and xylene/methanol (3:1) developers. Using IPA/water developer, the sensitivity of SML was improved considerably and found to be comparable to benchmark polymethylmethacrylate (PMMA) resist without affecting the aspect ratio performance. Employing 30-keV exposures and ultrasonic IPA/water development, an aspect ratio of 9:1 in 50-nm half-pitch dense grating patterns was achieved representing a greater than two times improvement over PMMA. Through demonstration of 25-nm lift-off features, the pattern transfer performance of SML is also addressed.     

Photocatalytic oxidation of ketones in the gas phase over TiO2 thin films: a kinetic study on the influence of water vapor

Photocatalytic oxidation of two ketones having different hydrophilicity, acetone and methyl isobutyl ketone (MIBK), over TiO₂ thin films supported on glass rings was studied under different relative humidity (RH) conditions. Adsorption isotherms of both ketones in the dark under different concentrations of water vapor were also measured and modeled considering a two-site Langmuir model. As expected, an increase in RH resulted in a decrease in the surface concentration of the organic molecules, but the photocatalytic oxidation rates did not show a parallel variation. In the case of acetone, almost total mineralization was achieved, and the kinetic constants obtained from fitting the data to the Langmuir–Hinselwood–Hougen–Watson (LHHW) model, were significantly larger in the presence of water vapor. Photocatalytic elimination of methyl isobutyl ketone (MIBK) is proposed to take place simultaneously by a direct oxidation route and by a sequential mechanism. Acetone is a stable intermediate in this last reaction pathway. Photodegradation of MIBK at different levels of RH was also modeled using LHHW kinetic expressions, and the rates obtained were slightly lower than those obtained for the photooxidation of acetone. However, a carbon balance was not achieved for MIBK, very likely due to the accumulation of partially oxidized products on the surface of the photocatalyst. The influence of water vapor on the photocatalytic oxidation rate of this larger ketone is more complex, and both inhibition and promotion effects can be envisaged. In addition, experimental results show that humidity exerts a significant influence in the mineralization efficiency of MIBK.     

乙二醇独乙醚-甲基异丁基酮-水三元非均相共沸物系分离研究

实验考察了液液萃取法、加盐分相法、共沸精馏法对乙二醇独乙醚-甲基异丁基酮-水( EC+ MIBK+ H2O)三元非均相共沸物系的分离效果.结果表明:以苯、甲苯、环己烷为萃取剂的液液萃取法分离效果较差;以K2CO3晶体为加盐相的加盐分相法,虽然可以取得较好的分离效果,但是不利于工业化生产;以甲基异丁基酮为夹带剂的间歇式共...     

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。     

国内甲基异丁基酮的生产情况及市场分析

甲基异丁基嗣主要用于溶剂和橡胶助剂领域,目前我国已成为甲基异丁基酮主要消费国.     

甲基异丁基酮的生产消费和发展趋势

阐述了甲基异丁基酮的主要用途、生产工艺、国内外消费市场及价格变动情况，对我国发展甲基异丁基酮提出建议。     

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。     

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。     

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。     

Droplet coalescence and breakage rates in a packed liquid extraction column

Coalescence rates for MIBK (methyl isobutyl ketone) droplets in water in a packed column have been measured directly using a novel colorimetric technique. Second-order coalescence and first-order breakage rate constants were derived from the results using a discrete population balance model and were correlated in terms of droplet diameter and dispersed-phase holdup. It is shown that the rate constants can be used to predict the steady-state droplet-size distribution and coalescence rates. They were also used in a theoretical study of mass transfer for a typical polydisperse system, which showed that repeated droplet coalescence and breakage leads to some reduction in column height.     

Preparation,characterization of MCM-56 and catalytic activity in one-step synthesis of MIBK from acetone

High crystalline MCM-56 was synthesized by dynamic method hydrothermally, and it was used as supports to prepare Pd/MCM-56 catalysts by ion-exchange method. The materials were characterized by means of N₂ adsorption, XRD, TEM, TPD. We found that as-made MCM-56 was made of very thin MWW-type layers with only one unit cell along the c direction. One-step synthesis of methyl isobutyl ketone from acetone was investigated over Pd/MCM-56. A conversion of 33.5% and a selectivity of 81.2% to MIBK were achieved. A stable MIBK yield was also obtained as well, maintaining 72 h of time on stream.     

巯基乙酸萃取工艺的研究

通过对若干种有机溶剂的比较,选定磷酸三丁酯(TBP)作为萃取剂,甲基异丁基甲酮(M IBK)作为稀释剂,对巯基乙酸(TGA)的萃取进行研究。同时考察了TGA浓度、萃取温度、pH等条件对TGA萃取分配系数的影响。实验结果表明,采用V(M IBK)∶V(TBP)=1∶9的混合萃取剂,控制V(有机相)∶V(水相)=1∶2,在室温下萃取TGA合成液两次,TGA萃取率达98.31%。萃取后有机相中含有无机酸杂质H2SO4和有机酸杂质二硫代二乙酸(DTDGA),可采用w(NaOH)=20%的水溶液洗涤去除。洗涤时控制n(NaOH)/n(DTDGA)=7,洗涤后无机酸杂质H2SO4去除率达100%,有机酸杂质DTDGA去除率达80.3%,TGA损失率2.6%,有机相中m(杂质)/m(TGA)=0.007 3。     

丙酮一步法合成甲基异丁基酮过程中精镏系统的研究

通过对甲基异丁基酮生产装置精馏系统的优化模拟 ,得到了整个流程的工艺设计参数。采用CY型高效丝网填料对原装置进行改造 ,改造后产品的产量、质量、收率等各项技术指标均达到设计要求 ,为建设万吨级装置奠定了技术基础     

MIBC生产技术研究进展及应用前景

综述了工业生产甲基异丁基甲醇(MIBC)的不同技术路线及研究进展。目前,经甲基异丁基酮(MIBK)加氢制备MIBC具有较好的应用前景,国内的MIBK生产厂可以在保证安全、有效生产的前提下,增设MIBC的生产装置,从而提高利润率,增强盈利及抗风险能力。丙酮一步法制备MIBC具有工艺简单、成本低廉的优势,可能是未来生产MIBC的研究热点,但需要加大力度研发新型高效多功能催化剂。     

丙酮一步法合成甲基异丁基酮

综述了丙酮一步法合成甲基异丁基酮的生产与研究现状。     

A rapid method for the determination of trace Cu and Fe in edible salad oil by graphite furnace atomic absorption spectroscopy

In the determination of trace amounts of copper and iron in edible salad oils by graphite furnace atomic absorption spectroscopy (GFAAS), an ashing method with low temperature oxygen plasma was used to effectively eliminate the interference of the organic matrix. Two sample preparation methods were studied, extraction with concentrated nitric acid followed by ashing with the low temperature oxygen plasma to determine the yield of extraction, and direct analysis of the metal content after dilution with methyl isobutyl ketone (MIBK). Results obtained from these methods were compared with the background absorbance by inductively coupled plasma-atomic emission spectroscopy (ICP-AES).