LAB REPORT SKKC 4761 SEPARATION PROCESSES LABORATORY II 2019/2020 – 04 EXPERIMENT 6 TITLE Double Effect Evaporation LAB INSTRUCTOR Dr Hashim Hassan SECTION 04 GROUP NO. 5 GROUP MEMBERS No. Name 1. SHAHIRAH BINTI SHAMSUDDIN A16KT0384 2. ZAHARATUL JANNAH BINTI SHAHARI A16KT0470 3. KAVILASHINI A/P MANIKAM A16KT0130 4 WONG JIA MIN A16KT0454 5 TWU LE YING A16KT0442 DATE OF EXPERIMENT : 01/10/2019 DATE OF SUBMISSION : 08/10/2019 GRADING SECTION Criteria Technical Aspects Matric Score / 5% Abstract / 10% Introduction Literature Review / 10% / 10% Methodology / 10% Results & Discussion Conclusion / 40% / 10% References / 5% Comment Overall Marks / 100% ABSTRACT Evaporation is a type of vaporization of a liquid that occurs from the surface of liquid into its gaseous phase at its saturation temperature. Boiling is another type of vaporization which is characterized by bubbles of saturated vapor forming in the liquid phase. Besides, evaporation is a kind of separation technique where it removes a liquid by boiling or vaporizing off some of the liquid in the feed. In this experiment, climbing film evaporator was used to separate the sugar and water from the sugar solution under single-effect evaporation. The two objectives in this experiment are to study the effect of operating temperature on the concentration profile of sugar solution and also the effect of feed flow rate on the final concentration of sugar solution. The sugar solution was prepared by dissolving 1 kg of sugar in 10 litres of water and served as the feed in the evaporator to undergo evaporation. Valves were closed every 5 minutes to collect the products at each different operating temperature, while every 5 minutes for 30 minutes for each feed flow rate to determine the refractive indices of the solutions. The results were then compared to the theoretical values from references to obtain the concentration profile of the sugar solution product. Based on the result obtained, when feed flow rate increased (6.48 L/hr, 9.72 L/hr and 12.96 L/hr) and the operating temperature was remained constant at 100ᵒC, the concentration of sugar solution decreased, which are 68.51%, 44.74% and 28.59% respectively. A higher volume of sugar solution and a lower volume of water were also obtained. The results were tabulated and graphs were plotted. Meanwhile, the discussion is also included in this report to support the results obtained. Some experimental errors and precaution steps were also mentioned in this report. 2 TABLE OF CONTENT TOPIC PAGE Abstract 2 Table of Content 3 1.0 2.0 3.0 Introduction 1.1 Background of Experiment 4 1.2 Problem Statement 5 1.3 Objectives of Experiment 5 Literature Review 2.1 Introductions 2.2 Basic Concept of Evaporation 2.3 Factors Affecting an Evaporation Process Methodology 3.1 Apparatus and Materials 9 3.2 Procedure 9 4.0 Results and Discussion 10 5.0 Conclusion 12 6.0 References 13 7.0 Appendices 14 3 1.0 INTRODUCTION 1.1 Background of Experiment Evaporation is a separation process used to concentrate aqueous solutions which involves removal of volatile solvent from an aqueous solution consisting of non-volatile solute by vaporization, in a vessel known as evaporator. Evaporation process begins with a liquid product and ends up with a more concentrated liquid as the main product. In some special cases, the evaporated, volatile component is the main product, for example in water desalination the vapors obtained by the evaporation process are condensed and used for drinking purposes. Similarly, the water that contains minerals is evaporated to obtain solid free water which can then be used in boilers. Air coil and liquid coolers are two main categories of evaporators used in industrial refrigeration. In the air coil, refrigerant passes through the pipes and air passes outside the tube. For efficient heat transfer fins attached to the external surface of pipes and air currents between the ribs. Besides, for natural circulation evaporators, forced circulation evaporators, rising film tubular evaporators and falling film tubular evaporators feed enters the bottom of the heating tubes and vaporization begins at that height within the tubes where the liquor temperature exceeds the boiling temperature at the existing pressure. As the liquor moves up inside the tubes, the liquor starts rapid boiling and additional vapor is produced and the velocity of the liquid vapor mixture increases. The vapor-liquid mixture then enters to the cyclone separator where they are separated. A climbing film evaporator is a specialized type of evaporator in which a thin film of liquid is passed over a rising and falling plate to allow the evaporation process to occur. It is an extension of the falling film evaporator and has application in any field where the liquid to be evaporated cannot withstand extended exposure to high temperatures, such as the concentration of fruit juices. The basic design of the climbing film evaporator consists of two phases. In the climbing phase, the liquid feed is heated by a flow of steam as it rises through a corrugated plate. In the subsequent falling phase, the liquid flows downward at high velocity under gravitational force. Evaporation and cooling occur rapidly in the falling phase. 4 The main advantage of climbing film evaporator is its short residence time. Since the liquid feed does not remain in the evaporator for long, this evaporator is suitable for heat or temperature sensitive material. Thus, this evaporator is used widely in food, beverages and pharmaceutical industries. Besides that, the colour, texture, nutritional content and taste of the liquid feed can be preserved too. Despite its functionality, this evaporator has a few drawbacks such as large energy consumption. 1.2 Objective of Experiment The objective of this experiment is: ● To study the effect of operating temperature on the concentration profile of sugar solution. ● 1.3 To study the effect of feed flowrate to the final concentration of sugar solution. Scopes of Experiment This experiment is conducted using is climbing film evaporator. 9.1wt% of sugar solution is fed into the evaporator to carry out the evaporation of water from the sugar solution to concentrate the sugar solution. The experiment is carried out at different feed flowrate and temperature to study effect of feed flowrate on the final concentration of sugar solution obtained. The volume and refractive index of product samples of water and sugar solution are measured at interval of 5 minutes for half an hour. The outcome of the result is discussed by the data collected. 5 2.0 LITERATURE REVIEW 2.1 Introduction Generally, evaporator is used widely in various process, including pharmaceuticals, food and beverages, chemicals, pulp and paper, polymers and resins, inorganic salts, acids, bases and a variety of other material. Evaporation is one of the process that can be used in order to concentrate the solution. According to Miyawaki et al. (2005), there are three methods always used in concentrating the solution which are reverse osmosis (RO),evaporation and freeze concentration. Based on these three methods, evaporation is the leading and earliest technology been used widely in various industry. There are various types and variations of evaporators, and the best for its application based on the product characteristics and desired results. The main advantage of climbing film evaporator is its short residence time. Since the liquid feed does not remain in the evaporator for long, this evaporator is suitable for heat or temperature sensitive material. Thus, this evaporator is used widely in food, beverages and pharmaceutical industries. Besides that, the colour, texture, nutritional content and taste of the liquid feed can be preserved too. Despite its functionality, this evaporator has a few drawbacks such as large energy consumption. 2.2 Basic Concept of Evaporation In evaporation, the vapour from a boiling point solution is removed and a more concentrated solution remains. In most of the cases, evaporation can be refers to the removal of water from an aqueous solution. According to Monceaux and Kuehner (2009), evaporation can be described as a process which involve the thermal energy in order to separate the substances, which the concentration of targeted solution is increased which caused by the separation of volatile component such as water in the original solution. Based on the difference in vapour pressure between the components, the volatile phase (water) is removed. 6 Evaporator is the device used in the evaporation process. The basic principle of evaporator is simple, which remove water from a solution or slurry through evaporation process. Evaporator is different from dryer because the concentrate discharge from evaporator is always in liquid phase. While, the discharge from a dryer is in solid form, usually a flowable powder or meal. The feed to an evaporator is always in liquid phase and still in liquid form even after the water is evaporated. The physical process of evaporation need the input of energy in form of heat in order to convert a liquid into vapour. Since most of the evaporators use the method of evaporation to remove water, so it is must for the evaporators have a source of heat to operate its system. The heat source for most of the evaporators is water vapour, either in the form of boiler steam or waste vapour from other processes. Besides that, evaporators require a means to transfer heat energy from the heat source into the evaporator liquid. Most of the evaporators use a tubular heater known as shell and tube heat exchanger for this purpose. In the shell part, water vapour is condensed on the outside of the tube which giving up its heat energy. The evaporator liquid, which is inside the tubes, absorbs the heat given up by the water vapour. Increasing in heat cause the water in the evaporator liquid to boil and produce bubbles of water vapour in the liquid. When these bubbles reach the surface of the evaporator and burst, the escaping water vapour carries some of the evaporator liquid with it. Some examples of evaporation are concentration of aqueous solution of sugar, sodium chloride, sodium hydroxide, glycerol, glue, milk and orange juice. For these cases, the concentrated solution is the desired product and the evaporated water is usually neglected. 2.3 Factors Affecting an Evaporation Process The physical and chemical properties of the solution being concentrated and the vapour being removed depends mainly on the type of evaporator used besides the pressure and temperature of the process. Several properties which affect the evaporation process is describe below. 7 1. Concentration in the Liquid The liquid feed to an evaporator is usually dilute, means low in viscosity, similar to that of water and relatively high heat-transfer coefficient are achieved. As evaporation proceeds, the solution may become very concentrated and quite viscous which lead to the mark drop in the heat-transfer coefficient. 2. Solubility When the solutions are heated and the concentration of solute increases, the solubility limit of the material in solution may be exceeded and crystals may form. This can limit the maximum concentration in solution which can be obtained by evaporation. Most of the time the solubility of the salt increases with temperature. So, during hot temperature, concentrated solution from an evaporator is cooled to room temperature and this can cause crystallization. 3. Pressure and Temperature The boiling point of the solution is related to the pressure of the system. The higher the operating pressure of the evaporator, the higher the temperature at boiling. Furthermore, as the concentration of the dissolved material in solution increases by evaporation, the temperature would rise. In order to keep the temperatures low in heat-sensitive materials, it is must to operate under 1 atm pressure which is under vacuum. 8 3.0 Methodology 3.1 Apparatus and Materials Climbing film evaporator, 250mL measuring cylinders, collecting jars, refractometer, 2kg of sugar, 20L of water 3.2 Procedures 1. Sugar solution was prepared using 2kg of sugar and 20L of deionized water. 2. The steam boiler was turned on. 3. The capacity of feeding pump was adjusted to 60% to manipulate the feed flowrate at 6.48 L/hr and the operating temperature was set at 115°C. 4. The feeding pump was turned on and the vacuum pump was switched on in order to speed up the evaporation process. 5. The product sugar solution and water condensed were collected separately by adjusting the position of the valves. 6. For collecting the product sugar solution sample, V7 was closed and V8 was opened simultaneously. At the same time, V9 was closed and V10 was opened simultaneously to collect the condensed water sample. 7. Then, the volume and refractive index of the collected product were measured. 8. The valve controlling steps (V7, V8, V9 and V10) were repeated every 5 minutes and the data collected was recorded. The same steps were repeated for 80% and 100% feeding pump capacity. 9 4.0 RESULTS AND DISCUSSION 4.1 Experimental Data Feed Flowrate (L/hr) Time (min) 6.48 5 10 15 20 25 30 5 10 15 20 25 30 5 10 15 20 25 30 9.72 12.96 Volume of Sugar Solution Obtained (mL) 170 100 130 130 130 130 350 270 230 230 230 230 460 450 450 400 430 440 Volume of Water Obtained (mL) 650 730 650 660 660 650 750 780 810 790 810 810 810 840 900 840 860 850 Refractive Index of Water Obtained, % 1.3337 1.3337 1.3334 1.3334 1.3334 1.3334 1.3336 1.3330 1.3337 1.3337 1.3332 1.3337 1.3337 1.3336 1.3337 1.3337 1.3338 1.3337 Sugar Solution Obtained Refractive Concentration Index, % ,% 1.3908 1.4135 1.4226 1.4301 1.4321 1.4403 1.4230 1.4076 1.4045 1.4031 1.4016 1.4029 1.3941 1.3812 1.3785 1.3785 1.3780 1.3775 Figure 4.1 Graph of sugar solution concentration versus feed flowrates 10 37.05 51.48 57.26 62.03 63.30 68.51 57.52 47.73 45.76 44.87 43.91 44.74 39.15 30.95 29.23 29.23 28.91 28.59 11 From the mass balance perspective, the volume of sugar solution and volume of water collected are inversely proportional to each other. When more water is being evaporated, less sugar solution is produced, resulted more concentrated sugar solution. This follows the material balance equation for an evaporator which is F= L + V, where F = Liquid feed flow rate L = Sugar solution flow rate V = Steam (water) flow rate Thus, the higher the operating temperature of the evaporator, the greater the volume of water being evaporated. Consequently, higher concentration of sugar solution is collected. According to Figure 4.1, the graph of sugar solution concentration versus feed flow rates shows that the sugar solution concentration is inversely proportional to the feed flow rate of the liquid sugar solution entering the evaporator. The concentration of sugar solution decreased when the feed flow rates increased. At faster feed flow rate, the residence time of the liquid sugar solution in the evaporator reduced. As a result, the heat transfer from the evaporator to the sugar feed solution become incomplete. In this context, incomplete heat transfer between the evaporator and the sugar feed solution greatly reduced the kinetic energy provided for the water molecules to break free from the hydrogen bonds, causing less water being evaporated and producing less concentrated sugar solution. Thus, at faster feed flow rate, the concentration of sugar solution become lower. As observed, the refractive index data for the water distillate are within the range of 1.3330 to 1.3337 which correspond to the theoretical water refractive index value, 1.333. This shows that the water distillate collected is comparably pure and does not contain any sugar. This confirmed no mistake is made while measuring the refractive index of the solutions. There are several precaution steps that should be taken into consideration to improve the accuracy of the experimental results obtained. Firstly, the time to turn off the valve before collecting the samples should be more constant and precise. This ensures 12 accurate amounts of samples are taken for the next measurement. Meanwhile, the sugar stock solution need to be prepared well before starting the experiment to prevent any insoluble sugar is found during the experiment. Lastly, the eyesight of observer should be perpendicular to the scale of the measuring cylinder when taking readings to minimize parallax error. 13 5.0 CONCLUSION Evaporation technique was used to separate both sugar and water in this experiment and the apparatus used was the climbing film evaporator. The objectives of this experiment are to study the effect of operating temperature on the concentration profile of sugar solution and the effect of feed flow rate on the final concentration of sugar solution. Based on the result obtained, when feed flow rate increased (6.48 L/hr, 9.72 L/hr and 12.96 L/hr) and the operating temperature was remained constant at 100ᵒC, the concentration of sugar solution decreased, which are 68.51%, 44.74% and 28.59% respectively. A higher volume of sugar solution and a lower volume of water were also obtained. The objectives of this experiment are achieved at the end of the experiment. 14 6.0 REFERENCES Badger, L. W., & Banchero J. T. (1955). Introduction to Chemical Engineering, McGrawHill, New York. Perry, R. H., & Green, D. (1988). Perry’s Chemical Engineers’ Handbook, 6th edition, McGraw-Hill. Geankoplis, C. J. (2014). Transport Processes & Unit Operations, 4th edition, Pearson Education Limited. Miyawaki, O., Liu, L., Shirai, Y., Sakashita, S., & Kagitani, K. (2005). Tubular ice system for scale-up of progressive freeze-concentration. J. Food Eng. 69(1): 107–113. 15 7.0 APPENDICES Appendix A: Concentration of sugar solution with respect to the refractive index Table A1 Refractive index for sugar concentration Sugar Concentration (%) Refractive Index (nD) 0 1.3330 5 1.3403 10 1.3479 15 1.3557 20 1.3639 25 1.3723 16 Figure A2 Graph of sugar concentration versus refractive index 17 Sample calculation: The linear equation of the graph plotted for sugar concentration versus refractive index obtained is: y = 635.69x - 847.07 For flow rate at 6.48 L/hr, the refractive index of sugar solution product is 1.4403nD. The sugar concentration corresponding to 1.4403nD is calculated by substituting the value into the equation obtained above. y = 635.69 (1.4403) – 847.07 y = 68.51 % Thus, the concentration of sugar solution is 68.51 %. Same calculation applied for the rest sugar solution concentration. 18 19