二元混合物塔顶累积全回流间歇精馏的最小气化总量

引　言80年代末 ,余国琮、杨志才等[1] 参照连续精馏开工过程的操作方法提出并实验证明了一种新的间歇精馏操作方法─—塔顶累积全回流间歇精馏(流程见图 1) .对于特定的分离任务 ,采用此操作方法间歇精馏与传统的恒回流比操作方法相比 ,能耗比较低 ,可望在工业生产上获得应用 .本文采用此操作方法推导了在理想操作条件下 ,间歇精馏二元理想混合物所需最小气化总量的计算方法 .Ｆｉｇ.1　Ｆｌｏｗｓｈｅｅｔｏｆｂａｔｃｈｄｉｓｔｉｌｌａｔｉｏｎｕｎｄｅｒｔｏｔａｌｒｅｆｌｕｘａｎｄｔｏｐａｃｃｕｍｕｌａｔｉｏｎ1,7—ｐｒｏｄｕｃ…     

二元混合物“全回流”间歇精馏的能耗

介绍了在理想操作条件下，“全回流”间歇精馏二元理想混合物量纲1最小操作总时间的数值计算方法.通过举例计算，比较了在理想操作条件下，“全回流”与部分回流间歇精馏二元理想混合物的能耗，得到了“全回流”间歇精馏适合于相对挥发度小、原料中轻组分的浓度低、塔顶产品中轻组分收率要求高而浓度要求低的分离任务的结论.     

恒回流比间歇精馏的最小回流比计算及其能耗分析

完善了采用恒回流比操作方法,在理想操作条件下间歇精馏二元理想混合物时,最小回流比的计算方法.分析了采用恒回流比操作方法间歇精馏二元理想混合物,在馏出液中轻组分的收率和平均浓度要求均高时,相对于恒馏出液组成操作方法能耗较高的原因.     

二元提馏式间歇精馏的优化操作与最小汽化总量

理想操作条件下二元提馏式间歇精馏优化操作的汽化总量与最小汽化总量的计算是约束函数优化问题。本文采用罚函数法,将此约束函数优化转变为无约束函数优化,并采用固定双步长因子梯度法数值求解该函数的极值。计算表明:固定双步长因子梯度法具有良好的收敛性,同时,降低分段数较多时,数值截断误差积累对计算结果的影响。二元提馏式间歇精馏优化操作较恒残液组成操作的能耗低的原因如下:在理论板数相对较少(接近二元提馏式间歇精馏恒残液组成操作所需的最少理论板)时,优化操作通过控制再沸比提高了能耗效率;在理论板数相对较多时,优化操作通过控制再沸比,在保证过程的能耗效率较高的同时,可尽可能快地将物料移出系统,减少了精馏过程中塔顶贮槽内液体的混合熵产。通过对计算结果的归纳与外推,得到了理想操作条件下理论板数为无穷多时二元提馏式间歇精馏优化操作再沸比的变化方式以及最小汽化总量的计算公式。     

恒全回流塔顶累积间歇精馏过程的研究

提出了一种过程始终为全回流操作的间歇精馏新型操作方式,其特征在于沿塔身不同高度设置有多个中间累积罐,操作中整塔始终处于全回流状态,每隔一段时间将下一级储罐内的液体转移至上一级储罐,塔顶储罐内液体作为产品转移到产品储槽。建立了该流程的数学模型并采用Matlab软件进行模拟,当目标产品浓度相同时,新操作方式的可以节省操作时间,在最优化的中间累计罐密集程度下,可节省50%左右,与具体操作参数相关;最后采用乙酸-水二元物系对该操作方式进行了试验验证,且整塔运行稳定易于操作控制。     

ChemCAD模拟分离混合二元酸二甲酯研究

采用ChemCAD软件对混合二元酸二甲酯的精馏分离过程进行模拟。首先选用简捷精馏模型分别对己二酸二甲酯和戊二酸二甲酯混合物,戊二酸二甲酯和丁二酸二甲酯混合物进行初步分离模拟,再选用联立矫正精馏模型进行两步间歇精馏模拟,得到合适的精馏条件。结果表明:精馏塔Ⅰ和精馏塔Ⅱ的塔板数均为22,塔顶压力为0.01 MPa,塔压降为0.001 MPa,再沸器温度小于423 K,进料口在塔板数12处,精馏塔Ⅰ最小回流比为2.42,精馏塔Ⅱ最小回流比为0.69时,进行模拟精馏,得到丁二酸二甲酯的纯度为99.60%,戊二酸二甲酯的纯度为99.61%,己二酸二甲酯的纯度为99.70%;根据模拟结果,采用精馏装置对混合二元酸二甲酯进行实验验证,实验结果与模拟结果相近。     

带有内部热集成的多储罐间歇精馏全回流操作

鉴于间歇精馏热力学效率低的缺点,提出带有内部热集成的多储罐间歇精馏全回流操作(IHIMVBD)分离二元混合物的新型操作方式。在该操作中,多储罐间歇精馏塔被同轴的夹套式再沸器环绕,利用安装在再沸蒸汽管线上的压缩机使精馏塔的操作压力高于夹套式再沸器,使热量通过精馏塔壁面从高压的精馏塔传向低压的再沸器,实现热量的内部集成。为了进一步提高热力学效率和经济效益,将塔顶蒸汽再压缩技术应用于IHIMVBD,构成强化的内部热集成多储罐间歇精馏全回流操作(Int-IHIMVBD)。该操作能额外利用被压缩的塔顶蒸汽的潜热供给塔釜料液再沸,实现塔顶蒸汽与塔釜料液的热集成。通过模拟分离乙醇-正丙醇的实例表明,相比MVBD和IHIMVBD,Int-IHIMVBD能显著提高分离过程的热力学效率和经济效益。     

双回流动态累积间歇精馏全过程的研究

在动态累积间歇精馏塔中,采用双回流动态累积间歇精馏操作对正丙醇-异丙醇二元混合物系进行分离研究。主要考察了操作时间对塔顶整个过程产品浓度、温度变化的影响,并与塔顶回流动态累积间歇精馏操作的分离结果进行了比较,以及过渡馏分阶段操作时间对塔釜正丙醇浓度及温度变化的影响,同时,又对正丙醇的回收进行了研究。结果表明,在同样的产品采出要求条件下,双回流动态累积间歇精馏操作时,随原料中异丙醇含量的增加,所需的操作时间越长,产品的纯度越高,收率越高;操作时间节省166 min,原料中异丙醇质量分数为30%的条件下,所得回收正丙醇的纯度达到91.22%,正丙醇的回收率可达62.93%,原料中异丙醇质量分数别为30%、50%、70%时对应过渡馏分持续时间分别为40、47、58 min;原料中异丙醇质量分数越大,所得回收正丙醇产品的量越少,正丙醇的纯度越低,回收率越小。     

真空间歇精馏分离橙花醇和香叶醇的研究

橙花醇和香叶醇是重要的基础香料,沸点差仅为2℃,具有热敏性。以往研究中应用减压间歇精馏分离橙花醇和香叶醇的混合物,一次精馏得到90%以上的产品收率低(仅为46%),且塔釜温度较高,操作周期长,不宜于工业生产。本文针对沸点差较小的热敏性物系,采用减压高效间歇精馏方法对橙花醇和香叶醇的混合物进行了分离研究。通过考察全回流时间、回流比、加热负荷和压力等操作因素对分离效果的影响,确定了适宜的操作条件,塔顶压力为600Pa～700Pa,塔压降为4800Pa～4900Pa,釜温在150℃～152℃之间,全回流6h,采用20 1,10 1,5 1的变回流比操作。实验结果显示,单塔精馏即可得到含量大于90%的橙花醇和香叶醇,收率在65%以上,提高20%无热分解现象,过程稳定,为工业生产奠定了基础。     

无累积罐循环全回流间歇精馏三温控制操作

提出了通过塔顶、塔中上以及塔中3个温度控制进行操作状态转换的无累积罐循环全回流间歇精馏控制方法,并以理想物系--乙醇-正丙醇混合物为分离物系进行了实验研究。通过实验确定了温度控制条件为当塔顶温度稳定后且塔顶和塔中上温差为0.3 ℃时变全回流为全采出操作,当塔中温度升高1.0 ℃时停止全采出转为全回流操作。同时还考察了在不同乙醇投料浓度条件下这种操作的运行情况,发现不同投料浓度对塔顶产品平均纯度的影响并不显著,基本能保持在0.99。最后在相同的投料浓度和操作条件下,对比了这种新型控制方式和双温度控制方式,结果表明三温度控制方式比双温度控制方式操作时间减少了23.3 min,分离效率提高了23.95%,产品浓度提高了1.06%,产品收率提高了1.08%。     

Numerical Modeling of Reacting Liquid Glass Layer in an Advanced Glass Melter

In the advanced glass melter small particles of batch materials are rapidly heated to glass formation temperatures while entrained in gas, and then deposited on a target surface. The resulting liquid slurry, consisting of sand, CaO, and MgO particles in the liquid formed by mixing of molten cullet and Na₂CO₃, flows down the center body. During this flow the solid particles dissolve in the liquid and diffuse to form glass. This paper describes a numerical model developed to describe the behavior of this liquid layer. The model is based on Navier-Stokes equations reduced for the case of a low Reynolds number liquid layer flowing under the action of gravity and shear from gases flowing on top. Experimental results agree with model predictions.     

Optimal programming of ideal and extractive batch distillation: single vessel operations

This work addresses the problem of optimal programming of multi-component batch distillation columns with a single vessel (batch rectifier, batch stripper, middle vessel and extractive middle vessel) so as to maximize an annualized profit function. A smooth price function is formulated for product valuation, allowing to release traditional purity constraints. The solution is the optimal batch policy of top/bottom withdrawals. A simplified cascade model is developed for separation calculations, offering several operational patterns. Ideal and non-ideal mixtures can be handled with this model that is proposed as a substitute for traditionally used Fenske–Underwood–Gilliland cascades. Batch separations of ideal quaternary feeds are optimally programmed for the first three operations aforementioned. The extractive middle vessel column was optimally programmed for production of anhydrous ethanol from hydrated, nearly azeotropic, alcohol with ethylene–glycol as entrainer. All applications considered fixed number of stages, heat duty, and, in the extractive system, fixed pump-around rate of entrainer.     

Shortcut Procedure for Inverted Batch Distillation Column (Ⅰ) Multicomponent Ideal System

Inverted batch distillation colunm(stripper) is opposed to a conventional batch distillation column(rectifier). It has a storage vessel at the top and products leave the column at the bottom. The batch stripper is favourable to separate mixtures with a small amount of light components by removing the heavy components as bottom products. In this paper, we are presenting a shortcut procedure based on our earlier work for design and simulation of the inverted batch distillation column, which is equivalent to the Fenske-Underwood-Gilliland procedure for continuous distillation. Given a separation task, we propose to compute the minimum number of stages(Nbmin)and the minimum reboil ratio(Rbmin) required in a batch stripper,which are the stages and reboil ratio required in a hypothetical inverted batch distillation colnmn operating in total reboil ratio or having an infinite number of stages,respectively. Then, it is shown that the performance of inverted batch columns with a finite number of stages and reboil ratios could be correlated in Gilliland coordinates with the minimum stages Nbmin and the minimum reboil ratio Rbmin.     

反置式间歇蒸馏塔的设计程序(Ⅰ)多组分理想物系

Inverted batch distillation column(stripper) is opposed to a conventional batch distillation column(rectifier). It has a storage vessel at the top and products leave the column at the bottom. The batch stripper is favourable to separate mixtures with a small amount of light components by removing the heavy components as bottom products. In this paper, we are presenting a shortcut procedure based on our earlier work for design and simulation of the inverted batch distillation column, which is equivalent to the Fenske-Underwood-Gilliland procedure for continuous distillation. Given a separation task, we propose to compute the minimum number of stages(Nbmin) and the minimum reboil ratio(Rbmin) required in a batch stripper,which are the stages and reboil ratio required in a hypothetical inverted batch distillation column operating in total reboil ratio or having an infinite number of stages,respectively. Then, it is shown that the performance of inverted batch columns with a finite number of stages and reboil ratios could be correlated in Gilliland coordinates with the minimum stages Nbmln and the minimum reboil ratio Rbmin.     

Untersuchung der batchweisen Azeotroprektifikation zur Trennung des Gemischs Essigsäure/Wasser

The aim of the present work is to investigate the suitability of the UNIFAC method to properly simulate the batch azeotropic distillation of a mixture of acetic acid, water, and ethyl acetate. A batch distillation including upstream countercurrent liquid‐liquid extraction was performed at pilot scale. A dedicated analytical method for fast and robust determination of top and bottom products was developed and presented. Experimental data were finally used for the validation of numerical predictions. It could be demonstrated that the UNIFAC method is applicable for the simulation of such a complex transient distillation process.     

精馏与盐效萃取偶合过程

设计了一种适用于从含水量较高的共沸液中分离有机溶剂的装置,该装置将精馏和盐效分相器结合起来,并带有中间储罐,其特点是：分相器可以将塔顶蒸出的共沸物中的大部分水除去,中间罐可以实现水从塔底除去。该装置上、下同时出水,有机溶剂浓缩在中间罐中。该装置大大缩短了操作时间,节约了能源。对该装置进行了数学模拟,与实验结果吻合较好。