Scaling Up Process Output of Monomer Reactor ...

Advanced Materials Research Vol. 748 (2013) pp 299-303 Online available since 2013/Aug/30 at www.scientific.net © (2013) Trans Tech Publications, Switzerland doi:10.4028/www.scientific.net/AMR.748.299

Scaling Up Process Output of Monomer Reactor Anika Zafiah M. Rusa, Muhamad Soqhimi Mohamad Isab, and NurulSaidatulSyida Sulong Department of Material And Design Engineering, Faculty Of Mechanical And Manufacturing, Universiti Tun Hussein Onn Malaysia, Parit Raja, 86400, Johor, Malaysia a

[email protected], [email protected]

Keywords: scale up, monomer reactor, waste cooking oil, pilot scale

Abstract. A monomer processing reactor is a device to process used cooking oil into new substance that can be used for other applications. In this study, used cooking oil was converted to monomer via simple reactor comprised of stirrer started with laboratory scale of 2L to 5L of monomer production. A scale up process is an important process for approaching industrial scale productions. The scale up process was increased to pilot scale before it reaches to industrial scale. The reactor is designed based on lab scale process for producing monomer from used cooking oil. The most important point of the device design is to produce larger amount of monomer compared to lab scale equipment. The device can produce 15liters of monomer per production. The monomer has the same properties and quality of monomer that were produced using laboratory equipment. Introduction Huge quantities of waste cooking oils and animal fats are available throughout the world, especially in the developed countries. Management of such oils and fats pose a significant challenge because of their disposal problems and possible contamination of the water and land resources. Even though some of this waste cooking oil is used for soap production, a major part of it is discharged into the environment. As large amounts of waste cooking oils are illegally dumped into rivers and landfills, causing environmental pollution [1], the use of waste cooking oil for monomer production is essential to the environment and society. Batch reactors are the most common type of industrial reactor. Reactants are charged to the system, rapidly mixed, and rapidly brought up to temperature so that reaction conditions are well defined [2].Observed reaction rates in small-scale reactors are often strongly influenced by reactor hydrodynamics and transport limitations. The designer must carefully monitor these effects when designing a commercial scale reactor [3].A major problem to restrict its commercial application is due to the difficulty in scaling-up the results from small laboratory batch equipment, such as stirred tank, to large continuous industrial unit. Often results from small-scale test units predict reactant conversion and space–time yield, which cannot be achieved when the equipment size is increased [4]. Scaling up reactors is important for engineers and it is the essential step for the realization and optimization of industrial plants. Scaling up is the synthesis of the phases for process development from the design of laboratory experiments and the derivation of kinetic correlation, to fluid dynamic experiments, mathematical modeling, design and operation of pilot and industrial plants. Laboratory reactors should not necessarily similar to industrial plants, but it has to be designed to give the best information about industrial plants. Experiments should be carried out sequentially and followed by statistical and mathematical modeling analysis in order to improve the quality and provide the first tools for scaling up. A pilot plant is used to test out the technologies needed for industrial scale. It is also need not be exactly the same ones employed in the laboratory, in order to point out those phenomena not present on laboratory scale. A pilot plant also need to prove that an existing laboratory scale unit yields the same results on a larger scale. A pilot plant also is important to evaluate product specifications and to set up automation and control system that will be ready for the industrial scale plants [5]. All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP, www.ttp.net. (ID: 103.31.34.2-29/12/14,08:45:36)

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Scale up and process development Scale-up or scale-down procedures are part of the integrated process development. The challenge is to find the optimum between the chemistry, the design, the EHS (environment, hygiene, and safety) compliance, and economic factors. This iterative process requires concept discrimination at the early stage of the process development. A direct transfer from laboratory scale to the industrial scale is rarely feasible. Generally, one or several scales between the lab and the industrial process may be used [6]. The monomer reactor processing was scale up from 5L productions to 15L productions. The processes of scaling up involve sketching and mechanical drawing of the reactor. The reactor was build according to the same feature of the 5L reactor. There are some features that were remodeled and modified for improvements. The scaling up process does not involve in the change of material for the vessel. The vessel was made of stainless steel to prevent the monomer mixture from sticking to the vessel. The volume of processing was increased, but some of the features were remained. The technical specifications were modified as the reactor needs to run higher amount of mixtures. The most important features that were changed are the power and speed of the motor, the baffled length, the controller and the heater for the reactor. For the design, the propeller shaft has a supporter to make sure that the rotations are balanced. The safety factor of the process also has been reviewed. 5 Liters reactor The design of 5L reactor consist of a motor, tank, propeller, inlet and outlet valve, control box, heater and body frame. It is does not came with wheel for easy placement and baffle for the mixing process. However, the reactor is not so heavy for easy movement. The design has eliminated many laboratory equipment and ease of handing. It also reduces the cost and time for the processing of monomer. The reactor is design to ensure bigger amount production of monomer than laboratory scale. This is the step for experimental scale where the reactor runs in the laboratory. Figure 1 shows the drawing and design of 5L reactor.

Figure 1: Schematic and transparency drawing of 5L reactor. 15 Liters reactor 15L reactor was designed based on 5L reactor. Some modifications were made for improvement from the processing and quality of the reactor. Basically, the concept is the same, but some adjustments were made. 15L reactor has bigger power electrical motor compared to 5L reactor. The

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inside of the tank is baffled, to help with the mixing process of the monomer. The outer tank was jacketed to prevent heat radiation and heat lost. This feature also for the safety of any person that operates the reactor from heat that radiates from the process. Safety factors are essential for bigger amount process. Some safety measures were taken such as a safety fuse for the motor and limiter control. The motor will shut down if it is too hot and the temperature inside the tank will be maintained at the desired temperature. The reactor was built with wheels so that it can be move where it is suitable to run the process. Figure 2 show the drawing and design of 15L reactor.

Figure 2: Schematic and transparency drawing of 15L reactor tank. Converting vegetable oil to monomer In polymer industry, vegetable oils which represent a major potential source of chemicals have been utilized as an alternative feedstock for monomers [7]. Recently, vegetable oil from Small Medium Entrepreneurs (SME) was successfully synthesis to produce a natural polyol in which hydroxyl group (OH) were required to react with isocyanate. Green monomer based on waste cooking oil from Small Medium Entrepreneur (SME’s) was prepared by using in house production of catalyst to generate the epoxides from unsaturated fatty compound which comprises the acid-catalyst ring opening of the epoxides to form polyols [8-9]. The vegetable oil was poured into the reactor and phase transfer catalyst was added into the reactor. The mixture was stirred for about 10 minutes at the temperature of 50ºC. After 10 minutes, catalyst, hydrogen peroxide and distilled water was added and the mixing was continued for 6 hours within the temperature range of 60ºC - 90ºC. After 6 hours, the mixture was cooled down for 30 minutes and the monomer produced from the process can be seen through the observatory glass at the outside of the reactor. The glass will show two layers of mixtures, that is monomer on the top and by product at the bottom of the reactor [10]. Results and discussion Vegetable oils have been successfully converted into monomer using both reactors. The monomer produced from both reactors had been analyzed by means of Fourier Transform Infrared (FTIR) spectroscopy. The FTIR represent a powerful tool for the characterization of polymer containing characteristic of functional group. The working wavenumber of the spectroscopy starts from 4000700 cm-1 and the resolutions of 32cm-1.

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Figure 3 shows the percent of yielding or conversion of bio-monomer for both reactors. The same volume of oils was used for the conversion process. Its shows different types of waste cooking oils of virgin oil (VO), popia oil (PO) and mixed oil (MO) were successfully converted into hydroxylated bio-monomers. The mass after the conversion process by monomer reactor were exceeded the original of mass oils of 210 gram. The highest yielding of bio monomer was based on the virgin palm oils (VO) whereby this oil contains more unsaturated fatty acids [7-10].

Figure 3: Conversion of 3 types of oils into bio-monomer

Figure 4: FTIR spectra of monomer produced from both reactors. Figure 3 shows the spectra of FTIR for the monomer produced from both reactors. The readings and numbers shows the results for the 15L reactor tank. FTIR spectra of the monomer from both reactors show the functional group at approximately the same at each peak. The IR absorption of the hydroxyl (O-H), alkynes(C-H), esters (C=O), alkyl halides (C-H), aromatics(C-H) function group are indicate in the range of (3400-3200cm-1), (3000-2850 cm-1), (1750-1735 cm-1), (13001150 cm-1) and (900-675 cm-1) respectively. From the FTIR spectra, hydroxylated monomer can be used to react with different types of crosslinker to form urethane linkage and it is called polyurethane. The versatility of polyurethanes has allowed the synthesis of different materials such as foams, coatings, adhesives, sealants, and elastomers. These materials can be used in fields as automotive, footwear, in construction as insulators, and most recently in medical devices. Polyurethanes have become one of the most used polymers due to their wide range of applications, properties and versatility. However, polyurethanes from vegetables oils are biodegradable and it is safer to the environment compared to synthetic petroleum based polyurethanes.

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Conclusion Scaling up process is a vital step to approach the industrial scale productions. Any development of a novel process that were once experimental and were done in lab scale shall undergo scaling up process before industrial scale take up. The scaling up process usually done in steps and the maximum scaling up depends on the results and analysis of the products. The output of the scaling up reactor must have similar quality and properties to the previous scale of production. Some rooms for modifications and improvement can and have to be made before the industrial uptake. This process plays an important role in designing a process. Acknowledgement The author would like to thank the Malaysian Government and University Tun Hussein Onn Malaysia (UTHM), Johor for supporting this research under Malaysian Technical University Centre of Excellence (MTUN CoE) research grant Vot C014. References [1] Arjun B. Chhetri, K. Chris Watts and M. Rafiqul Islam, Waste Cooking Oil as an Alternate Feedstock for Biodiesel Production, Energies (2008). [2] E. Bruce Nauman, Chemical Reactor Design, Optimization, And Scale-up, McGraw-Hill, (2002). [3] Daniel A. Hickmana, Meinolf Weidenbachb, Daniel P. Friedhoffa. A comparison of a batch recycle reactor and an integral reactor with fines for scale-up of an industrial trickle bed reactor from laboratory data, Chemical Engineering Science 59 (2004) 5425 – 5430, Elsevier. [4] Kai Zhang, Yulong Zhao, A scale-up strategy for low-temperature methanol synthesis in a circulating slurry bubble reactor, Chemical Engineering Science 61 (2006) 1459 – 1469, Elsevier. [5] Gianni Donati, Renato Paludetto, Scale Up Of Chemical Reactors, Catalysis Today 34(7: 483533), Elsevier, (1997). [6] Thierry Meyer, Scale-Up of Polymerization Process: A Practical Example(American Chemical Society, Switzerland, March 12, 2003). [7] Anika Zafiah, M.R.: Effect of Titanium Dioxide on Material Properties for Renewable Rapeseed and Sunflower Polyurethane, International Journal of Integrated Engineering (Issues on Mechanical, Materials and Manufacturing Engineering), Vol.1 (2009), pp.15-22. [8] Anika Zafiah M. Rus., Degradation Studies of Polyurethanes Based On Vegetables Oils. (Part I). Prog in Reaction Kinetic And Mechanism, Science Reviews, Vol. 33 (2008), pp 363-391. [9] Anika Zafiah M. Rus, Material Properties of Novelty Polyurethane Based On Vegetable Oils, The 11th International Conference on QiR (Quality in Research), Depok, Indonesia, (3-6 August 2009). [10] Anika Zafiah, M.R.: Degradation Studies of Polyurethanes Based on Vegetable Oils. Part 2; Thermal Degradation and Materials Properties, Prog. React Kinetic and Mechanism, Science Reviews, Vol.34 (2009), pp.1-43.

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Scaling up Process Output of Monomer Reactor 10.4028/www.scientific.net/AMR.748.299 DOI References [4] Kai Zhang, Yulong Zhao, A scale-up strategy for low-temperature methanol synthesis in a circulating slurry bubble reactor, Chemical Engineering Science 61 (2006) 1459 – 1469, Elsevier. http://dx.doi.org/10.1016/j.ces.2005.08.040