从异丙醇装置副产中分离精制异丙醚的工艺研究

采用萃取精馏和共沸精馏的试验方法,从异丙醇装置副产中分离精制异丙醚可以得到纯度大于99％的异丙醚和纯度大于99．5％的异丙醇,并且产率较高,具有明显的经济效益。     

从异丙醇装置副产中分离精制异丙醚的工艺研究

采用萃取精馏和共沸精馏的试验方法，从异丙醉装置副产中分离精制异丙醚可以得到纯度大于99％的异丙醚和纯度大于99．5％的异丙醇，并且产率较高，具有明显的经济效益。     

萃取精馏分离苯-异丙醇共沸体系的模拟

通过COSMO-RS软件计算,选择离子液体1-己基-3-甲基咪唑醋酸盐([HMIM]Ac)作为萃取精馏分离苯-异丙醇的共沸物合适的萃取剂。采用Aspen Plus流程模拟软件模拟苯-异丙醇共沸体系的连续萃取精馏过程。对两塔连续萃取精馏工艺过程,使用灵敏度分析工具优化,得出当回流比为1. 4、溶剂比为0. 365时,产品苯的纯度为99. 99%,异丙醇的纯度为99. 99%。此结果可为苯-异丙醇共沸体系的萃取精馏过程工艺设计提供理论基础。     

加碱萃取精馏制取无水叔丁醇

以乙二醇与KOH的混合物作萃取剂,采用加碱萃取精馏对85%叔丁醇进行分离,得到了纯度为99.5%的叔丁醇产品。设计了工艺流程,确定了操作条件,萃取剂可用减压精馏的方法回收,回收的萃取剂循环使用不影响分离性能。实验结果表明:加碱萃取精馏也是分离叔丁醇-水恒沸体系的有效方法。     

从异丙醇装置副产中分离精制异丙醚的工艺研究

采用萃取精馏和共沸精馏的试验方法,进行了从异丙醇装置副产中分离精制异丙醚工艺的研究,结果可以得到纯度大于99%的异丙醚和纯度大于99.5%的异丙醇,并且产率较高。     

异丙醇生产副产物中异丙醚的分离精制技术

采用萃取精馏和共沸精馏的试验方法,从异丙醇装置副产品中分离精制异丙醚．结果表明,以甘油为萃取剂,甲醇为夹带荆,可分别得到质量分数大于99％的异丙醚和质量分数大于99．5％的异丙醇,异丙醚收率为70．35％,具有明显的经济效益。     

头孢噻肟钠生产中甲醇、丙酮与乙酸乙酯混合溶媒的分离

通过萃取精馏、精馏对甲醇、丙酮与乙酸乙酯的混合溶媒加以分离,通过对生产数据的调整,确定了萃取精馏过程中混合溶媒与萃取水加入比例为1∶1,此条件下,萃取效果最好。萃取塔顶可以得到丙酮与乙酸乙酯和水的共沸物,塔底可以得到纯度为99.5%的甲醇。     

异丙醇-环己烷共沸物的分离与节能工艺研究

应用化工过程模拟软件Aspen Plus对异丙醇-环己烷最低共沸物系的连续萃取精馏过程进行了模拟与优化。通过Radfrac模块比较了不同萃取剂在相同条件下的分离效果,筛选出最佳萃取剂为乙二醇。运用灵敏度分析工具确定了最优工艺参数。采用双塔差压工艺进行节能改造,节能7.06%,异丙醇的纯度达99.96%,环己烷的纯度达到99.98%;萃取剂乙二醇的循环补充量为0.4741kg·h-1。     

萃取精馏分离丙酮-四氢呋喃的研究

为了分离丙酮-四氢呋喃共沸混合物,研究了萃取精馏在丙酮-四氢呋喃物系中的应用。通过溶剂选择原理初选出乙苯作为萃取精馏分离此共沸物系的溶剂,同时采用NRTL模型对常压下丙酮-四氢呋喃物系和加入溶剂乙苯后的汽液平衡进行模拟和实验验证,模拟结果与实验数据吻合较好。然后进行了间歇萃取精馏分离此共沸物的实验研究来进一步考察所选萃取剂的效果。结果表明:乙苯能够消除丙酮-四氢呋喃共沸物系的共沸点,采用有40块理论板的填料塔,回流比为5,溶剂摩尔比为2.5∶1时塔顶可以得到质量分数为99.34%的丙酮产品,说明采用乙苯作萃取剂分离丙酮-四氢呋喃共沸物是可行的。最后又对连续和间歇萃取精馏分离丙酮-四氢呋喃共沸物的流程进行了模拟,得到的工艺参数将为进一步的工业应用提供了理论依据。     

异丙醇-环己烷废液的提纯

对大学物理化学实验中的“双液系气-液平衡相图的绘制”实验产生的异丙醇-环己烷废液进行了分离提纯。先以水为萃取剂,对异丙醇-环己烷混合物进行萃取分离,再分别精馏提纯,得到纯度为99．492％的环己烷和纯度为98．710％的异丙醇。     

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.     

氨基磺酸催化合成苯甲醛乙二醇缩醛

以氨基磺酸为催化剂合成了苯甲醛乙二醇缩醛,考察了醛醇摩尔比,反应时间,催化剂用量,带水剂用量等因素对苯甲醛乙二醇缩醛收率的影响。结果表明：最适宜的工艺条件是：n（苯甲醛）：n（乙二醇）=1：1．5,催化剂用量占反应物总质量的1．5％,带水剂环己烷用量为16mL（占反应物总质量的2．18％）,反应时间1．5h,上述条件下,苯甲醛L--醇缩醛收率可达到83．73％。     

Design and control of reactive distillation for ethyl and isopropyl acetates production with azeotropic feeds

Reactive distillations for the production of ethyl acetate (EtAc) and isopropyl acetate (IPAc) are classified as the type-II process where the first column consists of a reactive zone and a rectifying section followed by a stripper [Tang et al., 2005. Design of reactive distillations for acetic acid esterification with different alcohols. A.I.Ch.E. Journal 51, 1683-1699]. Instead of using pure alcohols and acetic acid as reactants, this paper studies the effects of reactant purity on the design and control of reactive distillation. This offers significant economical incentives (by reducing raw materials costs), because ethanol forms an azeotrope with water at 90 mol% and isopropanol/water has an azeotrope at 68%. The purities of the acid is set to 95% for acetic acid (industrial grade), 87% for ethanol, and 65% for isopropanol. The results show that the total annual costs (TAC) increase by a factor of 5% for EtAc and 8% for IPAc production using reactive distillation. Next, the operability of the reactive distillations with azeotrope feeds is explored. Three disturbances, feed flow, acid feed purity, and alcohol feed composition, are introduced to assess control performance using dual-temperature control and one-temperature-one-composition control. Simulation results indicate good control performance can be achieved for reactive distillation with azeotropic feeds.     

TS-1催化丙酮氨氧化合成丙酮肟工艺研究

以钛硅分子筛(Ts-1)为催化剂,过氧化氢和丙酮为原料,催化氨氧化合成丙酮肟.对影响合成反应的多个因素进行了考察,合成条件经正交实验优化后丙酮肟产率有了较为明显的提高.结果表明:在反应温度65℃,搅拌转速320 r/min,质量分数30%过氧化氢水溶液滴加3.5～4.5 h,催化剂用量为丙酮质量的40%,n(丙酮):n...     

溶胶-凝胶法制备钛酸钡薄膜过程中溶剂的选择

合成透明稳定的溶胶对于制备优异电性能的BaTiO3（BT）薄膜是尤为关键的一步。以无水乙醇、异丙醇、乙二醇和乙二醇甲醚4种溶剂做对比,从合成溶胶的稳定性、表面张力以及制备出的BaTiO3薄膜的SEM等几方面比较了4种溶剂的优缺点,最后以乙二醇甲醚合成的溶胶最清晰、稳定,用此溶胶在Si（100）基底上得到了均匀无开裂的钛酸钡薄膜。     

10.8%精喹禾灵水乳剂的配方研制

介绍了10.8%精喹禾灵水乳剂的配方研制过程,即采用相转移法,以外观、乳化分散性、乳液稳定性、冷贮稳定性、热贮稳定性和常贮稳定性等为测定指标,通过对各种助剂(溶剂、乳化剂、增稠剂、抗冻剂和稳定剂)的选择,确定了最优配方:精喹禾灵10.8%,甲苯30%,Tween-8010%,黄原胶0.6%,乙二醇5%,稳定剂0.8%,消泡剂0.1%,纯水补足至100%。用上述配方所制备的水乳剂各项指标合格,在(54±2)℃的环境中热贮14d,分解率低于3%。     

农药液体制剂中5种助剂的气相色谱测定方法

本文建立了农药液体制剂中乙二醇甲醚、乙二醇乙醚、乙二醇甲醚醋酸酯、乙二醇乙醚醋酸酯、环己酮5种有害助剂的气相色谱法定量分析的方法。采用甲醇为溶剂,使用HP-INNOWAX毛细管柱,进样口和检测器温度为220℃,柱温采用程序升温进行测定。方法的线性决定系数大于0.9950,添加回收率在96.1%~102.2%之间,定量限(LOQ)为1.4~3.8 mg·L-1。采用所建立方法对市售的7种不同剂型的农药产品中5种有害助剂的含量进行了分析,环己酮成分在部分制剂中被检出。     

乙二醇双琥珀酸烷基聚氧乙烯醚双酯磺酸钠的合成及泡沫性能研究

采用乙二醇、马来酸酐和脂肪醇聚氧乙烯醚(AEO3)为主要原料,采用两步酯化反应和磺化反应,在催化剂的作用下,合成了一种阴非离子型双子表面活性剂。各步反应的最佳条件:酯化反应Ⅰ(反应温度120℃,马来酸酐与乙二醇的摩尔比为2.15∶1,催化剂用量2%,反应时间4 h);酯化反应Ⅱ(AEO3∶酯化产物Ⅰ摩尔比为2.10,反应温度180℃,催化剂用量3%,反应时间6 h);磺化反应(温度100℃,亚硫酸氢钠与酯化产物摩尔比为1∶3,催化剂用量1.5%,反应时间4 h)。产物的临界胶束浓度为0.17 mmol/L,γCMC为35.2 m N/m,浓度750 mg/L时,泡沫性能达到稳定。     

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.     

导电聚氨酯分散体的制备及应用

以聚乙二醇单甲醚(MPEG)为亲水单体,聚己二酸新戊二醇酯(PNA)、异佛尔酮二异氰酸酯(IPDI)为原料,通过丙酮法制备了聚氨酯分散体(PUD)。再以过硫酸铵为氧化剂,在PUD中氧化聚合PEDOT制备了导电聚氨酯分散体,并经IR、动态光散射和TEM表征,结果表明,导电聚氨酯复合材料形成了以PU乳胶粒子为核,导电聚合物PEDOT为壳的核壳形态,探讨了核壳粒子形成过程。利用自制的导电聚氨酯分散体配制得到了抗静电涂料,并成功应用于PET塑料基材。