Intensification of the Production of 2-Ethyl-Hexyl Acrylate: Batch Kinetics and Reactive Distillation

Author(s):  
Vivek D. Talnikar ◽  
Onkar A. Deorukhkar ◽  
Amit Katariya ◽  
Yogesh S. Mahajan

Abstract The reaction of acrylic acid and 2-ethyl-1 hexanol was explored in this work with the intent of process intensification. In order to assess the effect of important parameters on the course of reaction, this work initially conducted batch reactor experiments. Reaction conditions in the batch reactor for a specific conversion (~ 30 %) were obtained. A kinetic model was then obtained through regression to arrive at a rate expression that is later used in process development. Experiments were performed in the reactive distillation (RD) environment in batch mode, which showed substantial increase in conversion (~ 80 %) indicating the applicability of RD. Further, this work performed simulation in the RD environment to assess process intensification. Simulations show that it is possible to obtain complete conversion of the acid.

Author(s):  
Wentao Han ◽  
Zhenwei Han ◽  
Xuechao Gao ◽  
Zhou Hong ◽  
Xingang Li ◽  
...  

Ethyl levulinate, one of main derivatives of levulinic acid (LA), is of significant potential as platform chemicals for bio-based materials. The esterification of LA was generally carried out in a conventional batch reactor or in a conventional reactive distillation column. However, traditional methods are hard to deal with equilibrium limited reactions and azeotropic issues. Therefore, the reactive-vapor permeation-distillation (R-VP-D) process, which integrated reaction, distillation and membrane dehydration into one single unit, is proposed in this paper and validated in the pilot-scale experiments. A comparative study is made between a pilot-scale RD column with and without vapor permeation membrane module. Owing to the water-selective membrane and the ingenious design of related apparatuses, the R-VP-D process reveal a superiority in LA conversion of 21.9% maximum higher than RD without VP process and removing of product water about 53.6% from VP module, which indicates its promising industrial application in process intensification field.


Author(s):  
Timothy Aljoscha Frede ◽  
Marlene Dietz ◽  
Norbert Kockmann

AbstractFast chemical process development is inevitably linked to an optimized determination of thermokinetic data of chemical reactions. A miniaturized flow calorimeter enables increased sensitivity when examining small amounts of reactants in a short time compared to traditional batch equipment. Therefore, a methodology to determine optimal reaction conditions for calorimetric measurement experiments was developed and is presented in this contribution. Within the methodology, short-cut calculations are supplemented by computational fluid dynamics (CFD) simulations for a better representation of the hydrodynamics within the microreactor. This approach leads to the effective design of experiments. Unfavourable experimental conditions for kinetics experiments are determined in advance and therefore, need not to be considered during design of experiments. The methodology is tested for an instantaneous acid-base reaction. Good agreement of simulations was obtained with experimental data. Thus, the prediction of the hydrodynamics is enabled and the first steps towards a digital twin of the calorimeter are performed. The flow rates proposed by the methodology are tested for the determination of reaction enthalpy and showed that reasonable experimental settings resulted. Graphical abstract A methodology is suggested to evaluate optimal reaction conditions for efficientacquisition of kinetic data. The experimental design space is limited by thestepwise determination of important time scales based on specified input data.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Mathias Fink ◽  
Monika Cserjan-Puschmann ◽  
Daniela Reinisch ◽  
Gerald Striedner

AbstractTremendous advancements in cell and protein engineering methodologies and bioinformatics have led to a vast increase in bacterial production clones and recombinant protein variants to be screened and evaluated. Consequently, an urgent need exists for efficient high-throughput (HTP) screening approaches to improve the efficiency in early process development as a basis to speed-up all subsequent steps in the course of process design and engineering. In this study, we selected the BioLector micro-bioreactor (µ-bioreactor) system as an HTP cultivation platform to screen E. coli expression clones producing representative protein candidates for biopharmaceutical applications. We evaluated the extent to which generated clones and condition screening results were transferable and comparable to results from fully controlled bioreactor systems operated in fed-batch mode at moderate or high cell densities. Direct comparison of 22 different production clones showed great transferability. We observed the same growth and expression characteristics, and identical clone rankings except one host-Fab-leader combination. This outcome demonstrates the explanatory power of HTP µ-bioreactor data and the suitability of this platform as a screening tool in upstream development of microbial systems. Fast, reliable, and transferable screening data significantly reduce experiments in fully controlled bioreactor systems and accelerate process development at lower cost.


Author(s):  
Yogita P. Labrath ◽  
Prafulla V. Belge ◽  
Uma G. Kulkarni ◽  
Vilas G. Gaikar

Abstract The turmeric rhizome (Curcuma longa) contains curcuminoids embedded in the starch matrix. It is thus important to target starch hydrolysis to enhance extraction of curcuminoids. In the case of starch hydrolysis, α-amylase is more efficient when the starch is in a gelatinised form than when it is in its natural form. The present work includes hydrolysis of turmeric starch in its natural and gelatinised forms using α-amylase in hydrotrope solution (HS) and scCO2. The optimum rate of starch hydrolysis was obtained using 200 IU cm−3 of α-amylase, at reaction conditions of 6.5 pH at 328 K when 10% w/w of turmeric powder was stirred at 900 rpm in HSs. The hydrolysis in 15 MPa scCO2 at room temperature required a phase modifier and 40 min of residence time (RT). The enzyme treatment of turmeric powder in HSs increased the filtration rate for curcuminoid extraction (gelatinised and native) compared to untreated turmeric powder.


2021 ◽  
Vol 903 ◽  
pp. 143-148
Author(s):  
Svetlana Cornaja ◽  
Svetlana Zhizhkuna ◽  
Jevgenija Vladiko

Supported 3wt%Pd/α-Al₂O₃ catalyst was tested in selective oxidation of 1,2-propanediol by molecular oxygen. It was found that the catalyst is active in an alkaline water solution. Lactic acid was obtained as the main product of the reaction. Influence of different reaction conditions on 1,2-PDO conversion and oxidation process selectivity was studied. Partial kinetic orders of the reaction with respect to 1,2-propanediol, c0(NaOH), p(O2), n(1,2-PDO)/n(Pd)) were determined and an experimental kinetic model of the catalytic oxidation reaction was obtained. Activation energy of the process was calculated and was found to be about 53 ± 5 kJ/mol.


Author(s):  
Himangshu Mondal ◽  
Kanti Kumar Athankar ◽  
Kailas L. Wasewar

Abstract Biomass is an attractive target in process development for the emerging renewable resources based bio-refinery industry. Due to the ample range of application of acrylic acid, its production through bio-route received more awareness in scientific fraternity. In this view, an attempted was made to study the reactive extraction of acrylic acid with aliquat 336 in rice bran oil. Moreover, Box-Behnken matrix was employed to corroborate the effects of process variables viz. concentration of acrylic acid [CAA]aq, concentration of aliquat 336 [CR4N+Cl], and temperature on the extraction efficiency (η%). In physical extraction, average extraction efficiency was found in the order as: 43.55 > 35.36 > 29.14 at 303 K, 323 K, and 343 K respectively in rice bran oil. The correlation coefficient, R2 = 0.988 % indicates the appropriateness of proposed model to predict the extraction efficiency in terms of independent variables, and the predicted values were found in close agreement with that of experimental results. Further, R2(Pred) = 0.806 is in reasonable agreement with the R2(Adj) = 0.972. The optimum conditions for extraction of acrylic acid using aliquat 336 as an extractant in rice bran oil are [CAA]aq = 0.0.5 (mol/kg); [CR4N+Cl] = 1.98 (mol/kg); temperature = 323 K and the model predicted extraction efficiency 77.5 % was found to be an excellent fit with the experimental value 75 %. Further, number of theoretical stages was found to be 3 and S/F ratio 0.247.


2015 ◽  
Vol 13 (3) ◽  
pp. 389-393 ◽  
Author(s):  
Emine Sert

Abstract Within the framework of green chemistry, catalysts should be met different criteria such as biodegradability, recyclability, flammability, non-toxicity and low price. Acidic deep eutectic solvent (DES) have been synthesized for this purpose, by mixing para-toluene sulfonic acid and choline chloride. The catalytic activity of DES was studied in the esterification of acrylic acid with n-butanol. The usage of DES as catalyst is simple, safe and cheap. The effects of temperature, catalyst loading, n-butanol/acrylic acid molar ratio on the conversion of acrylic acid were performed. The batch reactor experiments were carried out at temperatures of 338, 348, 358 and 368 K, molar ratio of butanol to acrylic acid of 1, 2,3 and catalyst loading of 10, 15, 20 and 90 g/L. 90.2% of acrylic acid conversion was achieved at a temperature of 358 K and catalyst loading of 20 g/L. Reusability of DES was investigated. Reusability and catalytic activity makes DES efficient as catalyst.


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