Purification of tetrahydrofuran from its aqueous azeotrope by extractive distillation: Pilot plant studies

Deorukhkar, Onkar A.; Deogharkar, Bipin S.; Mahajan, Yogesh S.

doi:10.1016/j.cep.2016.04.006

Cited by 22 publications

(11 citation statements)

References 24 publications

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“…DMSO is selected as the entrainer. Deorukhkar et al 24 and Ghuge et al 8 have explored the suitability of DMSO and reported that it is efficient for the separation. The most suitable thermodynamic property model for this process is NRTL.…”

Section: Steady-state Designsmentioning

confidence: 99%

Comparison of Controllability Features of Extractive and Pressure Swing Distillations on the Example of Tetrahydrofuran Dewatering

et al. 2021

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The controllability study is an integral part of chemical process design. In this work, the controllability of two special distillation techniques, extractive distillation and pressure swing distillation, designed for the separation of azeotropic mixtures is investigated with dynamic tools. The control design interface of Aspen Plus and Matlab are applied for the modeling and evaluation of the two systems. Dynamic controllability indices are determined and aggregated in a desirability function. The results are compared to obtain efficient help for process design activity. The pressure swing distillation shows significantly better controllability features than the extractive distillation. The reason can be the fact that in the case of the extractive distillation, a third compound, the extractive agent, is added to the system to carry out the separation, therefore making the system more complex. As far as the selection of manipulated variables is concerned, in the case of the extractive distillation, the reflux flows should be preferred to the reflux ratios but in the case of the pressure swing distillation, the reboiler heat loads are preferred to the reflux ratios since those are closer to the controlled compositions. Both separation systems show worse controllability features if the product purity requirement is approaching to the pure products, that is, close to 100%. Although the energy consumption of the pressure swing distillation is higher than that of the extractive distillation, it has the inherent feature that it can be automatically heat integrated due to a column operated at high pressure and, as a consequence, higher temperatures.

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Section: Steady-state Designsmentioning

confidence: 99%

Comparison of Controllability Features of Extractive and Pressure Swing Distillations on the Example of Tetrahydrofuran Dewatering

et al. 2021

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“…Compared with studies on the measurements of vapour-liquid equilibrium (VLE) and the processes based on VLE data such as process feasibility, synthesis, design, optimization, control and so on, experimental studies on extractive distillation published in the open literature are scarce because conducting a very large number of experiments is neither practical nor economical (Deorukhkar et al, 2016). However, it is necessary to carry out experiments in a pilot plant to investigate the mass transfer efficiency and thus the rate-based model with the aim of predicting the performance of a real extractive distillation process.…”

Section: Experimental Workmentioning

confidence: 99%

“…Van Kaam et al (2008) verified their feasibility analysis by experiments for separating chloroform-methanol mixture in batch extractive distillation. Deorukhkar et al (2016) studied batch and continuous extractive distillation in experiments and found that dimethyl sulfoxide is a more appropriate entrainer than 1,2-propanediol for tetrahydrofuran dehydration. Zhan et al (2018) carried out experimentally batch extractive distillation for the separation of dimethyl disulfide from methyl tert-butyl ether by using diethylene glycol, dimethyl formamide and DMSO that had been screened from quantum mechanical calculations of interaction energies and dissipative particle dynamics of in the entrainers.…”

Section: Experimental Workmentioning

confidence: 99%

Review of extractive distillation. Process design, operation, optimization and control

Gerbaud

Rodríguez-Donis

Hégely

et al. 2019

Chemical Engineering Research and Design

211

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Operation and control Extractive distillation processes enable the separation of non-ideal mixtures, including minimum or maximum boiling azeotropes and low relative volatility mixtures. Unlike azeotropic distillation, the entrainer fed at another location than the main mixture induces an extractive section within the column. A general feasibility criterion shows that intermediate and light entrainers and heterogeneous entrainers are suitable along common heavy entrainers. Entrainer selection rules rely upon selectivity ratios and residue curve map (rcm) topology including univolatility curves. For each type of entrainer, we define extractive separation classes that summarize feasibility regions, achievable products and entrainer-feed flow rate ratio limits. Case studies are listed as Supplementary materials. Depending on the separation class, a direct or an indirect split column configuration will allow to obtain a distillate product or a bottom product, which is usually a saddle point of rcm. Batch and continuous process operations differ mainly by the feasible ranges for the entrainer-feed flow rate ratio and reflux ratio. The batch process is feasible under total reflux and can orient the still path by changing the reflux policy. Optimisation of the extractive process must systematically consider the extractive column along with the entrainer regeneration column that requires energy and may limit the product purity in the extractive column through recycle. For the sake of reducing the energy cost and the total cost, pressure change can be beneficial as it affects volatility, or new process structures can be devised, namely heat integrated extractive distillation, extractive divided wall column or processes with preconcentrator.

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“…In the chemical industry are numerous combinations of organic solvent and water, which are waste products in various processes and, in many cases, form an azeotropic mixture. For the separation of those mixtures, several techniques are used, including membranes, pressure swing distillation, and extractive distillation, because conventional distillation is not sufficient for azeotropic mixtures [2][3][4][5][6]. However, the achievement of high purity at low cost and energy consumption is still a challenge.…”

Section: Introductionmentioning

confidence: 99%

Zero-Discharge Process for Recycling of Tetrahydrofuran–Water Mixtures

2021

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The sustainable design of separation and polymer synthesis processes is of great importance. Therefore, an energy-efficient process for the purification of tetrahydrofuran (THF)–water (H2O) solvent mixtures from an upstream polymer synthesis process in pilot scale was developed with the aim to obtain high purity separation products. The advantages and limitations of a hybrid process in the pilot scale were studied utilizing an Aspen Plus Dynamics® simulation at different pressures to prove the feasibility and energy efficiency. For the rough separation of the two components, distillation was chosen as the first process step. In this way, a separation of a water stream of sufficient quality for further precipitations after polymer synthesis could be achieved. In order to overcome the limitations of the distillation process posed by the azeotropic point of the mixture, a vapor permeation is used, which takes advantage of the heat of evaporation already used in the distillation column. For the purpose of achieving the required low water contents, an adsorption column is installed downstream for final THF purification. This leads to a novel hybrid separation process that is energy efficient and thus allows also the use of the solvents again for upstream polymer synthesis achieving the high purity requirements in a closed-loop process.

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Purification of tetrahydrofuran from its aqueous azeotrope by extractive distillation: Pilot plant studies

Cited by 22 publications

References 24 publications

Comparison of Controllability Features of Extractive and Pressure Swing Distillations on the Example of Tetrahydrofuran Dewatering

Comparison of Controllability Features of Extractive and Pressure Swing Distillations on the Example of Tetrahydrofuran Dewatering

Review of extractive distillation. Process design, operation, optimization and control

Zero-Discharge Process for Recycling of Tetrahydrofuran–Water Mixtures

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