= suddy oy GY. = vs a \siien™ EVAPORATION THE PRACTICE — SteveSrec~ ‘Sugar Technology For Students EVAPORATION THE PRACTICE Prepared by G R E Lionnet Study Text 6 Published by G R E LionnetPublished by G RE Lionnet 25 Haleric Rd Durban North , 4051 KwaZulu Natal Rep of South Africa First published 1999 Copyright © 1999 GRE Lionnet Printed in Durban by GRE Lionnet ISBN 0-620-24197-7 ‘This text or any part thereof must not be reproduced in any form without the ‘written permission of the publisher. ‘This text forms part of a sugar technology study programme, The complete list of units in the programme appears at the end of this text. , new study units and other information, please write to GRE Lionnet, 25 Haleric Rd, Durban North, 4051, KZN, RSA.SEPARATORS |e EQUIPMENT KESTNERS ROBERTS CONDENSERS — FALLING FILM PLATE CONDENSATES INCONDENSABLE dS GASES fe 1 > CONTROL TECHNOLOGY Lo He | ENTRAINMENT ENERGY FOULING PINCH BLEED SCALE CLEANING |CONDENSATE | | MECH CHEM1. INTRODUCTION A general introduction to evaporation has been given in Study Text 5, Evaporation: The Fundamentals, That unit covers basic concepts dealing with energy, heat, and multiple effect evaporation. Various calculations are given in details. Finally, the chemistry involved with evaporation is discussed. For many years Roberts vessels and Kestners were the main types of evaporators used in the sugar cane industry. There has, however, been considerable developments recently, and a number of designs newto the cane industry, have been tested with cane juices, and some have been introduced on the industrial scale. A section on equipment is found in this Study Test, titled Evaporation: The Practice. Considerations particular to the cane sugar industry have always formed an important part of this study programme. This approach continues with evaporation, and the section titled The Technology is an important part of this Study Text \ Finally, the bibliography, for both Study Texts, is given at the end of this unit. equipment : New designs ‘The Technology Bibliography2,THE EQUIPMENT 2.1 Evaporators 2.1.1 Long tube climbing film Long tube climbing film evaporators have been used mostly as first effects in the cane sugar industry. They are often called Kestners, after their inventor, Paul Kestner. ‘The main advantages of the Kestner are its short residence time, its ability to contain much heating surface in a single vessel, its high coefficient of heat transfer and low levels of temperature differences. It consists of long vertical tubes inside a cylindrical shell. As many as 5000 tubes may be found within a single shell. The liquor to be concentrated is fed to the bottom of the tubes, where itis heated by steam condensing inside the shell. As vapour is formed in the tubes, it carries the liquor up the tube as a thin film against the tube wall. Heat transfer is favoured by the decreased distance between juice and wall, and by the high juice velocities. At the top of the tubes, the mixture of concentrated juice and vapour exits and is separated in a separator, usually of the tangential type. ¥ Lr Kestners‘The tubes are 6 to 10 metres long, 7 metres being common in South Africa, and 27 to 51mm in diameter, 50,8mm being found generally in South Africa, with a wall thickness of 1,2mm. Stainless steel tubes are preferred since they are not subject to steamside corrosion and are longer lasting, particularly if mechanical cleaning is used The separator in the cane sugar industry is generally located outside the evaporator itself. It consists of two sections, a lower one in which juice collects and is withdrawn to feed the next vessel, and an upper cone through which vapour is withdrawn. This upper section often contains an entrainment separator, usually a wire mesh pad. The diameter of the separator depends on the entrainment device used, and is usually similar to that of the evaporator vessel. The liquid feed should be distributed evenly below the bottom tube plate. Recent work in South Aftica has shown that there are two basic requirements for the feed to a Kestner. The first is to have single phase feed in the feed ring, that is to have liquid only, with no flashing; this ensures even distribution of the feed to all the tubes. Secondly, enough juice must be available to ensure that the feed ring is operating at design capacity. As far as feed temperature is concerned, itis believed that it should be approximately 1°C below that the boiling point of the juice at the vapour pressure of operation. The lid is detachable, to facilitate access for cleaning. A safety device is essential to prevent removal of the lid while there is still positive pressure in the vessel. Experimental work in pilot plant has shown flow throughputs of 25 to 140 kg/hr/tube to be possible, as first effect. In South Affica, 75 kg/hr/tube is the average in industrial first effects, while about 42 kg/hs/tube are found in second effects. Experimental work has shown that, in first effects, the throughput should not fall below about 60 kg/hr/tube for good performance, in terms of heat transfer coefficient Heat transfer coefficients (HTC) in industrial Kestners has been measured at 2,3 kW/m/°C in first effects, and 1,8 kW/m’/°C in second effects, Juice residence times in Kestners has also been measured. In first effects a time of 2,4 minutes is considered short, being about 15% of that in Roberts vessels. Values of 4 to 5 minutes have also been measured. 3 Tabes Feed Feed throughput Residence timeFinally mechanical cleaning is possible but becomes a strenuous undertaking as the number and length of the tubes increase. Chemical cleaning is also possible. 2.1.2 Roberts vessels ‘One of the main differences between Kestners and Roberts vessels is the tube length, In Roberts, tubes vary from about 1,9 m to 2,8 m, with a diameter of 38 to $1 mm. There is no juice/vapour separator associated with Roberts vessels. The vapour space of the vessel itself acts as a disengaging space and a height of about 3 to 5 m between the juice surface and the dome is common. A rule of thumb is that the height of the cylindrical part of the vessel should be about twice the length of the tube. exyoanns Ceaning Roberts Disengaging space‘The diameter of the vessel has an effect on entrainment since vapour velocity is affected by the cross sectional area Juice feed is normally through a feed ring, inside the vessel, with slots. Again there should be no flashing in the feed ring. The calandria is where the heat transfer takes place. The distribution of steam or vapour into the calandria should be as uniform as possible, and bafiles may be used. The downtake returns the boiling juice to the base of the vessel. Its diameter varies from 1/4 to 1/8 of the vessel diameter. Some vessels do not have downtakes; there is then no provision to return the juice to below the calandria and it must be assumed that the tubes which are boiling less efficiently than average act as down comers. There are two basic types of downtakes, the sealed downtake and the open downtake. Typical arrangements are shown below. Fred ring (CalandraAn entrainment separator is essential. It can be located in the top of the vessel or consist of mesh, or baffles, arresters in the body itself. In most evaporators the tubes are arranged in a staggered configuration, which permits the greatest number of tubes per unit area of tube plate, for a given distance between the tubes. This staggered arrangement is shown below. on QW ope tare osItis possible to calculate various ratios concerning tube arrangements in tube plates. All the following calculations are based on the diagrams on the previous page. ‘The four quarters of the tubes inside the parallelogram ABCD have an area equal to 77/4. ‘The corresponding area of tube plate is equal to the area ABCD. This will now be calculated. Using geometry Sin 6 = height P and height = 7 pe base = px Cos 60 = 0,5p ‘Area of plate ABCD Let K, be the ratio of area of holes to that of the total plate, Then area of holes ~ total plate areaAgain referring to ABCD, the area of the holes is md/4, while the 3 total plate area is ~~ p?. Then It is now easy to show that [Relainship betneen pic and tube diameter p=0,952 In industrial evaporators K, is approximately equal to 0,5. Then p= 14d that is the pitch of the tubes is about 1,4 times their diameter. We can also calculate X, the plate distance between tubes. Then X=p-2r =p-d that is Relatonship between X and ‘ube diameter iB‘Typical values for the heat transfer coefficients in Roberts vessels, and the juice and vapour temperatures, are shown in the following The residence time in Roberts vessels usually ranges from 5 to 10 amimutes. This can vary considerably and tracer tests ae needed when precise values are required Operating juice levels in Roberts vessels should be kept about half ‘way up the first sight glass, which normally corresponds to about 50 mm above the top tube plate. Finally, cleaning can be done mechanically or chemically. 2.1.3 Falling-film, tubular, evaporators Falling-flm, tubular, evaporators are popular in the beet industry, but applications in the cane industry have been slow. When used with ccane, the choice seems to have been based on energy considerations. This type of evaporator consists of a cylindrical vessel with the feed being spread, at the top, on a vertical bundle of tubes, by means ofa juice distributor, Juice then flows as a film down from the top to the bottom, with the vapour also flowing from the top to the bottom Thus both juice and vapour travel in the same direction, The concentrated juice and the vapour reach the base of the vessel and the vapour exits through a separator.Schematic diagram of tabular falling Sm evaporstor ‘The tubes are usually made of stainless steel, with a diameter of 38 Toes to 51 mm, and are 7 to 10 m long. Itis generally recommended that a wetting rate of 12 to 15 kg of juice per hour, per cm of tube be provided The juice distributor is an important part of the evaporator, and its ce ditbator design is vital to the operation. The distributor must not be blocked by suspended matter, for example scale, and juice velocities are important. Many designs are available and both steady and uniform flow is essential. A nozzle may replace the distributor and this is being evaluated in South Africa. ‘The separator can be incorporated inside the vessel or can be a — situated outside the evaporator itself Centrifugal or gravity separation may be used. A pump may be used to ensure correct flow, through recirculation. “are The heat transfer coefficient has been found to be about 2,4 kW/m?/°C, with cane juice, in a clean evaporator used asa first effect. After about 3 weeks of operation the HTC decreased to about 1,4 -10-kW/m? - The residence time is short, with work in India showing times of 0,5 to 0,6 minutes, but other workers quote values around 2 minutes. In South Africa little to no inversion has been found to occur. Cleaning must be by chemical means One such vessel has been operating in South Aftica and the experience (Rousseau ef al., 1995) shows promising results. A second evaporator is being installed. 2.1.4 The plate evaporator This is a different concept, not utilising tubes as such, The heat exchange surface is in the form of plates or cassettes, Both rising and falling film configurations are available. The plates can be inside a pressure vessel, or an external separator may be present. Again this design is popular in the beet industty where significant energy savings have been achieved through its application. The plates are usually about 0,6 mm wide with plate gaps of 10mm. ‘They are made of stainless steel, and gaskets are fitted between them, Plate area is about 2,6m?. The recommended wetting rate is 16 rm? per hour per 100m’ of area, The heat transfer coefficients in a second effect at 3,5 kW/m’/°C, were about 40% higher than found in Roberts vessel. The general consensus is that HTC values are high under optimal operating conditions, but are sensitive to control, fouling and general ‘operations. Retention times, found with beet juices, were short at claimed values around 30 seconds, These times are stated to be about 1/10th those found in Roberts vessels, for the beet industry. Plate evaporators have a number of special requirements: + The gaps between the plates are small. The feed juice must therefore be free from suspended matter. In the cane industry sieving or filtration may be needed. -l- Retention tome Residence time+ Itis critical to have uniform and steady feed distribution, at the designed flowrate, Juice flow control must be good. + Cleaning must be by chemical means, and must be efficient. Opening the heater for physical cleaning may damage the gaskets which are expensive. 2.2 Entrainment separators Entrainment occurs in nearly all processes involving gas/iquid contacting. It can be reduced by proper design and operation, but cannot be totally eliminated. Recovery devices, called entrainment separators, are therefore installed in evaporators to recover the entrained liquid. There are four main types of separators: + Centrifugal separators + Zigzag baffles + Impingement separators + Wire mesh pads 2.2.1 The centrifugal separator Centrifisgal force is used to throw the entrained droplets against an ‘outer wall where they collect, drain, and are returned to the vessel. Series of vanes or circular flow channels are used to force the vapour to flow ina circular path. These separators are usually situated in the dome of the evaporator. 2.2.2 Zigzag bafiles ‘These are a specific case of the impingement type of separator. They consist of series of parallel plates with bends. They are located across the cross-sectional area of the evaporator body. They are sensitive to -12- ‘Maln types of separatorsthe vapour velocity. Metal or plastic may be used for construction. ‘Schematic diagram ofa zlesag bafle 2.2.3 Impingement type As with the zigzag baffle, the impingement separator causes the separation of the liquid droplets. Schematic diagram of an Impingement separator2.2.4 Mesh pads Multiple layers of crimped, knitted mesh can act as an impingement separator. They are typically 10 to 20 em thick, and the mesh density can be changed. They come in segments and, contrary to zigzag baffles, can be made to fit a vessel of any shape. They can however foul and plug; a strict washing programme is necessary. 2.2.5 Washing arrangements In inal effect evaporators entrainment can be high due to high vapour velocities. If mesh separators are installed, washing is essential Experience in South Aftica shows that the following conditions may be used. Wash water temperature should be about 80°C, about 50 / of water per m’ of mesh are required, and a 5 minute wash every hour was adequate. This resulted in a mesh separator needing no removal for more than three month of operation. Steam or vapour may also beused for cleaning mesh separators. Two cleaning arrangements are shown schematically below. “14 Schematic dagram ofa mesh ina separator (Cleaning mesh separators(Cleaning of a meh separator with Tot water (Cleaning with vapour2.3 Condensers ‘The condenser is a heat exchanger, between the vapour and the cold water. This exchange will be more efficient as the contact between the vapour and water is more intimate. Counter current, rain tray type condensers are well utilised in the South African industry. Some design details are as follows. Vapour velocity is about 60 m/s; injection water velocity is around 1,5 m/s, and the air velocity is 12 ays. A perforated plate distributes the water; it usually has holes of about 12 mm diameter, with an average sized condenser requiring 2000 to 3000 holes. A splash plate is used to even out the water distribution. A schematic diagram is shown below. — T| -16- an tray condensers2.4 Condensate ‘There are two different conditions for the removal of condensates. ‘The calandria pressure can be above atmospheric pressure, in which case gravity may be used, since the condensate will flow freely. The pipe must not however be empty and thus allow steam or vapour to be lost. A steam trap is necessary. Thisis a device containing a float, which will open only when water reaches a given level, Then an equilibrium is reached and the float opens to let only water escape. The calandria pressure can be at sub-atmospheric levels. A number of devices may be used : + Sealing legs, as shown schematically below. c a) 7 — L, LJ | ] mame isa | ‘VESSEL WITH SEALING LEGS coeur +g —_ ‘The calandria of the 4* effect will be at the same pressure as the vapour of the 3 vessel, say 50 to 52 kPa absolute. This corresponds to a head of water of about 5 m, which with a 25% safety margin requires a leg of about 6 m; one needs a vertical distance of 6 m between the bottom tube plate of the 4" calandria and the top of the weir in the last compartment. This does not cater for accidental high -I7- (Calandria above atmospheric pressare Steam trap Sealing legsvacuum levels and the literature recommends about 10 to 11 m. This is often a practical problem in terms of space. ‘The three condensates are at different temperatures and thus should discharge in three separate wells, This prevents accidental flashing if the hotter condensate reaches the highest vacuum leg. + Siphon. Siphons pass condensates from one calandria to the next and recover the flash. A U-tube or inverted siphon is used Length and height must again have a generous safety margin, This can once more cause practical space problems. + Flash pots. These are small vessels situated below the evaporators, in which flash takes place. They do not require the vertical space of the two previous devices but need relatively complex piping. They should have sight glasses to allow visual inspection of what is happening inside them. 2.5 Incondensable gases Incondensable gas vents in the calandria should be located as far as possible from the steam or vapour entry point into the calandria. The pipe should start about 100 mm, atleast, from the base of the tube plate, to avoid contact with condensate For calandrias where the pressure is above atmospheric, incondensable gases are allowed to escape to atmosphere through a regulating valve. Flow’is set to allow a small wisp of steam to be seen escaping continuously. For calandrias under vacuum, the incondensable gases are led to the vapour space of the same vessel. The gas vents and pipes from successive vessels must be made progressively larger because of the accumulation of gas in this system. As a rule of thumb, one can use the following -18- Siphons lash pots (Calandria above atmospheric prewure-19- 1* vessel 13 mm pipe ~ 2° vessel 13 to 19 mm 3" vessel 19 to 25 mm 4° vessel 25 to 32 mm.3. THE TECHNOLOGY 3.1 Energy Many cane factories diversify their operations, depending on local conditions. Thus, back-end refining, bagasse exports to by-products, the production of electricity for the grid or for irrigation, can be major considerations. These increase the demand for the self- generation of energy, while often reducing the bagasse available for steam generation. Asa consequence it is often necessary to increase boiler capacity and to burn fossil fuel; at the same time the amount of steam for sugar processing must be reduced as far as possible. Reid and Rein (1983) give detailed energy balances for a modern South African factory, High pressure steam % cane is about 48%, for a mill providing fibre for by-products while burning a minimum of supplementary fuel. The major user of exhaust steam (203 kPa; 121°C) is the evaporator station, consisting of a quintuple; of the 306 tons of exhaust produced per hour, the evaporators consume 276 tons or about 90%. Thirty seven tons of V1 (164 kPa; 114°C), and 215 tons of V2 (130 kPa; 107°C) are bled per hour. The following three aspects of technology are relevant to energy savings in the cane sugar industry + Pinch technology. This can be used to assess the thermal efficiency of the evaporator station. Pinch technology has been quoted (Singh et al,, 1997) as being an efficient tool to do so. There is no doubt that new evaporator concepts and designs are being adopted in the cane sugar industry because of energy considerations. + Vapour bleeding. Vapour bleeding is a well established process for the efficient utilisation of steam. Normally in the cane sugar industry, only vapour 1 and 2 are bled. They feed juice heaters and the pans. Vapours from 3" and 4* effects are at relatively low temperatures and would require large surface areas for heat transfer. + Condensate management, Condensates are utilised in two main ways, to recover energy. Routing condensates to the next calandria recovers energy through flash, The complete recirculation of condensates in this way, for a quadruple effect, would give about 5% more evaporation. The use of condensates as a source of hot -20- Practical considerations ‘Steam tothe evaporntrs Vapour bleeding Condensate utilisationwater in the factory is the second, indirect way, of saving energy. The most important use is as boiler feed water; here the early, relatively uncontaminated condensates are selected First effect condensates may be sent to the boiler water feed tank, via steam traps, or they are sent via steam traps to the second vessel flash pot, any excess is then sent to the boiler feed water tank Second effect condensates are sent via steam traps to the 3% effect flash pot, with any excess to the boiler feed water tank or to the factory hot water tank. Third effect condensates are sent via steam traps to the flash pot and calandria of the 4" effect. Any excess is sent to the factory hot water tank, Fourth effect condensates are sent to the factory hot water tank. ‘ All condensates sent to boiler feed water are tested in line for conductivity, to be rejected as feed water ifthe conductivity indicates a possibility of entrainment of sugar. 3.2 Kestners ‘The use of long tube, climbing film evaporators (Kestners), as first and second effects is well established in South Africa. Their large capacities, coupled with short residence times, allow high evaporation. rates and efficient vapour bleeding, Recently much work has been done to optimise the operation of Kestners in South Aftica. Two main conclusions have been reached + Feed flow rate is possibly the single, most important ‘operational parameter. + Fouling of the tubes is the practical limit to good performance. Both these concepts are illustrated in the following figure, based on the pilot plant work done mostly by Walthew (1995, 1996). a Condensate from : Tetect tetect efter ‘Tes for entrainment ‘Tube sealingaan a ~ 3 2 #25 = 2 is Oo O18 = 1 05 20 40 60 80 100 120 FEED RATE (kg/hr/tube) For Kestners as first effects, a minimum feed rate of 60 ke/hr/tube is essential. Based on tube diameter, this corresponds to 3,8 kg/hr/em of perimeter, for a tube of 50,8 cm diameter. Its interesting to note that the heat transfer coefficient (HTC) does not decrease as flow Tate increases. In the South African industry, for 50,8 mm tubes, the range of flow rates varies from about 30 kg/hr/tube or 1.9 kg/hr/cm of perimeter, to 82 kg/hr/tube (5,2 kg/hr/cm). The average for eleven 1” effects Kestners was 63 kg/hr/tube (3,9 kg/hr/cm), which is just about the minimum recommended. For Kestners as 2™ effects, an average given in the literature is 42 kg/hr/tube (2,6 kg/hr/om perimeter for a 50,8 mm diameter tube) ‘These findings have prompted at least three South African factories to install juice recycling on their Kestners. A connecting pipe has been installed with a non-return valve, between the juice outlet from the I" effect separator, and the feed line to the 1* effect evaporator. The practical objective has been to obtain 72 ke/hr/tube. It is essential for the feed flow rate to be steady. Recycling does not “225 “Minizam flow rate for I ffcct Kevtners Feed recycling in Kestnersimprove the HTC directly but creates operational stability and reduces fouling, Good feed distribution has been found to be a prerequisite for efficient operation. Recent work by Walthew (1996)and mathematical modelling by Peacock (1997) have shown that the feed should not flash in the feed ring. Feed temperature should be 1,5 to 2°C below the expected boiling point of the juice; flashing seems to disrupt even distribution. It should be noted however that the feed temperature must not be too low since boiling must start within a short distance up the evaporator tube. James ef al, (1978) query whether Kestners should not be used as later effects. They support this claim with calculations which seem to. favour Kestners over Roberts as later effects. 3.3 Roberts vessels ‘ Roberts vessels tend to be taken for granted. In South Affica little work has been done recently with these evaporators, particularly when compared to Kestners. It should be noted that the single phase feed recommended for Kestners does apply to Roberts also. Investigations done in 1981 (Smith and Taylor) have shown that very low pressures in the last effect are in fact detrimental, reducing HTC values, due to viscosity effects. Evaporation can decrease by about 10%. The results of some of their calculations are shown in the following figure, and it is evident that the optimum pressure is about 16 to 20 kPa absolute, corresponding to 55 - 60°C. 2. Feed distribution Feed temperature Feed temperature ‘Presnre in las effect10 15 2 s 20 38 Last effect pressure (kPa ebs) 3.4 Falling film, tubular ‘The falling film, tubular evaporator has been intgoduced to the cane sugar industry basically from an energy saving point of view. It is claimed that it allows high temperatures but with short residence times. The literature quotes the following residence times : Effect i] 2 | at | 4* | se Residence time (min) | 1,2 | 14 | 1,7 | 22 | 41 It is also stated that, with cane juice, the flow rate should be at least 200 kg/hr/tube, or for tubes of 50,8 mm diameter, about 12 kg/hr/em of perimeter. These are high flow rates when compared to those recommended for Kestners. ‘Two tubular falling film evaporators operate in South Africa, as I and 2" effects. Inversion across the vessels has been found to be low. Juice recycling is vital to ensure the correct wetting rate. Operation and control have been said to be trouble free. 3.5 Plate evaporators Again the use of plate evaporators has been driven by energy 24 eed flow ratesconsiderations. The results obtained in the recent, and first, installations in the Southern African industry have been less clear than ‘was the case with the falling film, tubular evaporators. A number of concerns were envisaged + The effect of fouling under local conditions was unknown. + Cane juice is more turbid than beet juice and tends to contain more particulate matter. Sporadic carry over of clarifier muds does occur. + Operating conditions in terms of flow control is not always as good as required. Possibilities of dry out periods are very real. It was clearly evident from pilot plant work in a local factory that uniform and steady juice distribution was vital. Generally the rates required were around 15 tons per hour per 100m’ of plate area. Good heat transfer coefficients were obtained, with high juice throughputs. The results obtained with three new industrial plants were mixed. In one factory where the evaporator was installed recently, the results were seen as promising although the evaporator has operated for a short period of time only. Inthe other two factories serious problems arose, through poor juice distribution, caramelisation, cleaning difficulties, and desiznicapacity problems 3.6 Heat transfer coefficient values A summary of heat transfer coefficients (kW/m?/K) measured in various evaporators operating in the Southern African industry is given below. 1,8-2,3 - 26 1,0-2,4 18 19 2,5-3,5 . - 16 43 - - 09 0,6 : festee| - 06 05 : -25- Application with cane juice3.7 Control of evaporators Evaporator control may involve the following major variables : * Clear juice feed rate to 1" vessel + Steam flow rate or pressure to 1* vessel. + Liquid level in evaporators. + Final syrup brix, + Absolute pressure in last effect. The contro! philosophy will also depend on the type of the evaporator, for example Kestners, Roberts, etc, and for Roberts vessels whether they have open or sealed downtakes. Generally very steady conditions of juice flow, steam supply and vacuum are prerequisites to successful evaporator control In Kestners, liquid level is not usually controlled. For a 1* effect Kestner, the Roberts 2™ effect can be used to control the flow to the Kestner. Unsteady flows, or large fluctuations in vapour being bled, for example when a batch pan stops or starts, can cause oscillations. ‘These are made evident by pressure swings, with the vessel boiling and not boiling in turn, and by large ejections of juice into the separator. The practice of recycling the feed should help in eliminating this problem. Finally, the use of neural networks has recently been proposed for evaporator control. 26.3.8 Evaporator scale ‘The formation of scale in evaporators, also called evaporator fouling, is a major cause of poor heat transfer in the cane sugar industry. AS a result of this fouling either + the evaporator station is over designed to allow vessels to be taken off-line for cleaning, or + the factory must stop crushing at regular intervals, to allow the vessels to be cleaned. 3.8.1 Mechanisms of scale formation Scale formation in evaporator tubes is 2 complex process. The following mechanisms can be involved. + Concentration process. As water is evaporated, solubilities are reduced until precipitation takes place. The most soluble species, and those present at the lowest concentrations will be found as scale, in the later vessels. Generally the higher the syrup brix, the more scale is produced, It is accepted that pH will also affect the solubilities. + Chemical reactions. High temperatures and retention times will cause chemical reactions to take place. Sucrose can caramelise, and the monosaccharides can decompose to form organic acids, these in turn react with calcium ions, resulting in the formation and precipitation of organic calcium salts. + Particle deposition. Cane juice contains much suspended and colloidal matter. The effects of suspended matter is not clear, it may act as nuclei for the crystallisation of various species, it may attach itself to the tube wall and encourage deposition of scale. Itis believed that juice velocities in the tube, and pH are important. The state of the fube surface, on the juice side, has been considered. Tests were done in a pilot, two tube, evaporator, where one of the tubes was highly polished, by a commercial firm specialising in this type of work, while the other was used asis. Juice was concentrated from 20 0.60 brixin 100 hours, with recycling. No difference could be found, either in terms of HTC (3,8 kW/m??°C, for either tube), or in terms of fouling resistance (1,8 and 2,0 m°C/kW, for the polished and unpolished tubes respectively) -27- Practical impact of evaporator ‘sealing ‘Concentration process Particle deposition+ Operational factors, This is possibly the most important factor in cane sugar factories. Low and/or erratic juice flow rates result in severe fouling. In the worst cases, dry-out occurs and tubes or plates are blocked, It has been well demonstrated that steady operations, with the correct juice flow rate, reduce fouling and allow longer periods of operations before cleaning is required. 3.8.2 Chemical composition of scale 3.8.2.1 Sampling Sampling evaporator scale is not easy, particularly with respect to representativeness. When mechanical cleaning is used, some dissolution may take place, while the sodium hydroxide used in chemical cleaning could leach out some of the scale constituents. Finally, in wet scales, fermentation can occur and the acids formed could change the composition. 3.8.2.2 Analytical techniques + Drying, The scale sample is dried at 110°C, crushed and subdivided. + Ashing. A sub-sample is ashed at 1000°C; this gives a loss on ignition; only the oxides remain and the loss is based on this procedure, + XRF. X-ray fluorescence is used on another sub-sample, to yield information on the inorganic elements, for example SiO,, C20, MgO. + XRD. X-ray diffraction is used to identify the crystalline phases, both organic and inorganic, Thus, calcium oxalate, for example, will be differentiated as either the monohydrate or dihydrate; calcium carbonate crystallises in three different forms, which can be identified. + HPLC. High pressure liquid chromatography is used for organic acids + Conventional analyses. These are used as required, for specific information -28- XRDA calculation is done to balance the calcium found by XRF and that accounting for the calcium phosphates and oxalates. Excess calcium is normally left over after the calculation, and this is reported as “free” CaO. This extra calcium is thought to originate from clarifier mud catry over. 3.8.2.3 The chemical composition of scale in Southern Africa Over the past few years a large number of evaporator scale samples has been analysed in South Africa, mostly through the work of Walthew (1995;1996). Work has also been done in Australia by Crees et al. (1992). These results may be summarised as follows. * Impact of clarification. The process used for juice clarification will have a fundamental influence on the composition of the scale. Sulphitation, for example, will result in much calcium sulphate in the scale; defecation on the other hand results in the presence of calcium phosphates, Silica, and the tatal calcium content, however, seem to stay more or less constant, + Organic species. Sugar, sometimes caramelised, and other ‘organic species, may be trapped within bulky calcium phosphates, in earlier effects. Oxalates, usually as calcium oxalate, CaC,O,2H,0 or Ca C,0,H,0, are formed in later effects. Aconitic acid, a rare scale component, as calcium-magnesium aconitate, has sometimes caused major problems, due to difficulties in removing it + Inorganic species. The main inorganic species are calcium, magnesium and phosphates. Calcium phosphate species include Ca,(PO,),, an amorphous calcium phosphate, and Ca,,(OH),(PO,), a crystalline hydroxy apatite. Silica originates from the cane itself, being attached to the fibre. It is extracted from the cane, during milling or diffusion, with temperature and more particularly pH, increasing its extraction. Silica can also be introduced in the raw house when refinery sweet waters, which have circulated through diatomaceous earth filter aids, are returned. Very generally the distribution of scale in an evaporator tail depends on the position of the vessel. Many factors come into play, particularly whether hydroxy apatite (Ca,o(OH),(PO,),) is present or not, There is much variation but general trends in South Affica are shown below. -29- Et of claiiation Orginicspeces8 PERCENT OF DRY SCALE Ss 8 3.8.3 Methods to reduce fouling ‘As mentioned earlier, the impact of fouling on evaporator performance can be severe. Procedures to reduce, or even eliminate, fouling have therefore been investigated. + Removal. Species such as calcium, which cause scale, can be removed from the juice. Chemical precipitation, ion exchange, filtration, etc., during, after, or to replace clarification, are being considered. Calcium can be removed by the softening process, that is by replacing it with Na* or K’. Pilot plant work in South Africa (Thompson, 1994) has shown that nearly all the calcium and magnesium may be removed from clear juice. The scale formed in the pilot plant evaporator tubes had the composition shown below. sio, | cao | mgo | PQ, Now 1 2 4 24 fe 1 1 0 1 -30- RemovalUnfortunately the silica content is not reduced-by softening or by the usual defecation process. With softening, silica could become the ‘major scale species, causing it to be difficult to remove, since SiO, does not respond well to chemical or mechanical cleaning, + Antiscalants. A number of products are available commercially. They act as crystal habit modifiers, as complexing agents, or as dispersants. As yet, they have never produced spectacular results, in South Africa. They have, however, caused scale to be softer and thus easier to remove mechanically. Crystalline species in the scale may have been reduced, but no effects on the heat transfer coefficients has been seen. + Physical methods. These have not been successful generally. The techniques tested have included the use of spiral turbulence promoters, inserted in the tubes; of ultrasonic devices, and of magnetic devices. * Changes in operation. On the short toynedium term, these certainly offer the best possibilities to reduce evaporator fouling, Most importantly, juice flow rate to the evaporator must be at the required level and must be steady. There must never be fluctuations which could cause tube dry out; mud carry over must be eliminated; pH control must be good. These are basic requirements in any modem cane sugar factory and will go a long way in reducing fouling, 3.8.4 Fouling resistance The concept of a fouling resistance can be used in more fundamental studies of fouling, A fouling resistance, R,, is defined by equation 3.8.4.1 where U, and U, are the heat transfer coefficients (kW/m?/°C) after an operating time of t (s) during which fouling occured, and with 31. Physical methods Goo operation control Definition of fouling resistanceclean tubes, respectively. As usual U = oom where Q is the heat transferred (kJ/s), A the heat transfer area (m?), and dT the temperature difference (°C). R, is then the fouling resistance in m°CikW. The concept is used in making broad comparisons between evaporators. Say we have an evaporator which has been thoroughly cleaned and we measure the heat transfer coefficient (HTC) as it starts operating. We obtain an HTC value of 4,1 kW/m’/°C. The same vessel operates for two weeks after which time its HTC is now 3,5 kW/m?/°C. Then, using equation 3.8.4.1 : 14 35° ar ®% and R, is equal to 0,04 m’°C/kW. This quantifiés the fouling of that evaporator under the conditions of operation. Walthew (1996) gives values of R, for evaporators in Southem Africa, as shown below. The type of evaporator, its position in the tail, the geographical area from which the cane originates, and the climatic conditions all influence the fouling factor. = 1 2,5-3,0 r 04 a 0,2-03 ~ fe = on 0,1 32. Bxample of he calculation of the fouling factor ‘Values of fouling factors in ‘Southern Afien3.9 Evaporator cleaning Awide range of optionsis mentioned in the literature for the cleaning of evaporators. Practically, only two approaches remain, namely mechanical cleaning, with rotary scrappers, usually under wet conditions, and chemical cleaning, almost always involving the use of sodium hydroxide solutions. Whatever the option, evaporator cleaning has the following requirements : + It must be completed within the time available through the factory scheduled shut down. There is less urgency if vessels can be taken off line individually. In some cases a factory may have two extraction lines and two evaporator tails; then one line and one tail may be off line, without the whole factory being shut down, + The cleaning process must restore the heat transfer coefficient to an accepted level ; * Costs must be considered. 3.9.1 Mechanical cleaning Rotary scrapers, or brushes, on a long, flexible, electrically operated drive are used, The cutters are loosely mounted and centrifugal force provides the pressure on the tube surface. This approach copes with variations in tube diameter. The use of water assists in softening the scale and washes it away. ‘The advantages of this method are that its cost is generally lower than that of other options; it can utilise unskilled labour, and many vessels can be cleaned simultaneously, depending on the availability of labour and equipment. It is, however, an unpleasant operation in term of human comfort, and it may not always restore the heat transfer coefficient to its clean tube level. Tube damage is possible and the method does not deal well with hard scales. Visual inspection of whether the tubes are clean or not is difficult and needs long experience for good judgement. In South Africa mechanical cleaning is still cheaper than chemical cleaning. -33- “Mechanical and chemical options Practical requirements of ‘Caporator cleaning Wet scraping / brushing Advantages and disadvantages3.9.2 Chemical cleaning In most cases sodium hydroxide is used; itis sometimes followed by a second chemical, usually an acid. Recently (Walthew ef al., 1997; Peacock ef al., 1999), two approaches have shown promise; the first involves the use of a wetting agent to improve the efficiency of the sodium hydroxide solution, thus allowing a reduction in its concentration; the second has revived the interest in the use of chelating agents such as ethylenediaminetetrancetic acid (EDTA), and of equivalent, but cheaper, chemicals. The following practical details apply to the use of sodium hydroxide solutions + Strength. Practical considerations such as handling difficulties, and the possibility of gelling, limit the concentration of sodium hydroxide that can be used, to 30 - 40 % (mass NaOH to ‘mass solution), ‘ + Temperature. Observations in South Afiican factories show that cleaning improves as temperature rises, Usually a temperature of at least 90°C is needed, + Agitation. The sodium hydroxide solution can be used to flood the tubes or can be sprayed onto them. If flooding is used, then boiling is necessary and this provides the agitation, If spraying is used, which requires a smaller volume of solution, then nozzles are needed and about 0,5 to 1,0 Vmin/tube must be circulated by pumping. This corresponds to about 0,5 to 1,5 V/min/m? heating area, Generally flooding, with boiling, results in better cleaning + Time. A minimum of 3 hours contact time is needed. The sodium hydroxide attacks the organic species and silica in the scale. It is however not very efficient with respect to oxalates and phosphates. Once the scale has been physically disrupted by the sodium hydroxide, agitation can break it up and causes it to be removed from the tube. Sodium hydroxide is not corrosive to metals but its chloride content needs to be watched because of its effect on stainless steel. It has been noted that sodium hydroxide can cause metal embrittlement. -34- ‘These of NaOH Concentration ‘Temperature TimeThe disposal of spent sodium hydroxide solutions can be a severe problem in the cane industry. This is one of the points which needs careful consideration before this chemical is chosen for chemical cleaning. Chemical treatment of the spent NaOH is receiving attention in South Africa, but no obvious solution is apparent; it remains a subject of much research. A typical analysis of spent sodium hydroxide solution shows about 27% NaOH, 4% Na,CO,, 2,4% SiO,, 0,5% PO,, 0,3% CaO, and 66% water and others, all expressed as mass on mass solution. Recent work in South Africa (Walthew, 1997) shows that the concentration of sodium hydroxide solutions can be reduced, without, loss of cleaning efficiency, if a wetting agent is added. Results obtained in a pilot plant evaporator are shown below, where the concentrations of the sodium hydroxide solutions (mass on mass solution) is indicated. When a wetting agent was added at the concentration recommended by the manufacturer, the strength of the sodium hydroxide solution could be reduced to 4% (mass NaOH on mass solution) but the cleaning efficiency was excellent. These results need to be confirmed on the industrial scale. ° 05 1 15 2 25 TIME (hours) 35: Disposal of spent NaOH “The we of meting agents “The impact of a wetting agent on ‘leaning with NaOH (Pir plant sate)Acids can be used, being more effective against oxalates and phosphates. Both sulphuric and hydrochloric acids have been mentioned in the literature, at concentrations varying from I to 4%, at 60 to 80°C, for I to 6 hours. Both these acids must be inhibited Inhibition prevents the acid from affecting brass, iron, mild steel, etc. Usually organic compounds are added to the acid, as inhibitors. The organic molecule must have a polar group which attaches itself to the metal surface; the rest of the organic molecule then forms a monolayer coverage and protects the metal. The polar group doesnot bind to the scale, which can then be attacked. Phosphoric acid has been used in South Africa, Sulphamic acid, which has the advantage of being available as a dry powder, has been found to be efficient at attacking scale. It is however quite expensive; it decomposes at temperatures above 70°C and cannot therefore be used above that temperature. Chelating (Greek chele : claw) agents, such as ERTA can be used to remove calcium and magnesium. EDTA has six donor atoms ( 2 nitrogen and 4 oxygen) and this allows it to wrap itself around a Ca™* ion to form a very stable complex. EDTA has been used at concentrations of 4 to 5% (mass EDTA to mass solution). The sodium salt of EDTA is also compatible with an alkaline environment; this makes it suitable as a follow up after the use of sodium hydroxide solutions. Cost can however be a problem. Sodium glutamate is being investigated as a possible substitute for EDTA. The following procedures, among others, have been used in Southern Affica : + For tubular evaporators. 10 to 15% sodium hydroxide, plus 0,2% wetting agent. Boiled for 3 hours + For plate evaporators, 10 to 15% sodium hydroxide, plus 0,2% wetting agent. Boiled for 6 hours. Then flush with water and circulate 6% phosphoric acid solution at 80°C for 2 hours. The efficiency of the chemical cleaning procedures depends on many factors, some of which cannot be controlled while others are unknown, It is necessary to proceed cautiously when this type of evaporator cleaning is introduced for the first time; the concentration of the sodium hydroxide solutions, temperatures, agitation and -36- Acs and inhibitors ‘Salphamic acid Dra Pracedares nied in South Attica (Concentrations : mass to masscontact times should be set at the higher levels. Experience may then be used to optimise the procedures, both in terms of cost and of cleaning performance. -37-3.9.3 Steamside cleaning - Fouling on the vapour/steam side of the calandria is usually caused by the action of heat on organic materials such as traces of lubricants in the steam, or entrained sugar and other juice constituents. In South Africa Lewis et al. (1978) describe a number of methods to clean the vapour side of calandrias. Two commercially available products were mentioned. Organic acids such as acetic of formic, at Concentrations of 2% (mass / mass water) plus 0,5% (mass / mass water) of a non foaming detergent may also be used. Power paraffin in water has been used. Finally, diluted molasses has been allowed to ferment in the vapour space, over a long period, such as the off crop. 3.10 Entrainment ‘The entrainment of organic matter, mostly sucrose, into condensates impacts in two main areas. Firstly, there is a loss of sucrose which impacts on recovery directly; the entrained sugars will also cause problems in terms ofeffluent treatment. . scondly, entrainment affects the quality of the condensate with respect to its use as boiler feed water. There is therefore a need to prevent entrainment as far as possible, and to monitor the levels which will occur even with the best prevention measures. 3.10.1 Entrainment monitoring The monitoring of organic matter in raw house condensates used for boiler feed water requires a well designed conductivity system, and 2 dumping facility, on all condensates lines that supply the boiler feed water tank. Most of the entrained organic species, including sucrose, other than salts, have negligible conductivities. Their presence is inferred through the conductivity of the salts, both organic and inorganic, which are also entrained with the organic contaminants. The ratio of organic matter to inorganic species varies and conductivity set points need frequent and individual calibrations. In refineries, where the liquor purities are very high, conductivity cannot be used. Total organic carbon analysers are used, but these are costly and need relatively long analysis times which requires large -38- Causes (Cleaning chemicals (Conductivity and damping tems (Caltration Refineriescondensates storage volumes; dumping can be-wastefl Monitoring entrainment from a suerose loss point of view, is usually based on a programme of sampling and analysis. Two main approaches may be used. Firstly, samples of water are taken at points where specific streams meet; ifthe mixed condensates or waters show unduly high levels of sugar, the various individual streams are sampled and analysed, to identify the source of the problem. The other approach involves the use of quick, non quantitative analytical methods, which can show only whether sugar is present at a known minimum level or not. Again, should the result be positive, special sampling and quantitative analytical procedures are started. There are two main types of entrainment. The first is a sudden upsurge of juice, with flashing, due to a sudden increase in vacuum. Large quantities of sugar may be lost and, if the monitoring system is not well run, the loss may be missed. The second process is the continuous removal of smaller quantities of juice. Although less ramatic, this type of entrainment can be neglected and can cause low but continuous contamination of the boiler feed'water. 3.10.2 Quantification of entrainment Humm in 1979 and Lionnet in 1984 have measured entrainment in ‘cane sugar factories. Both authors show the importance of vapour velocities. Some results are shown below. 1010 40 21010 | 2 effect, Roberts 10 to 40 10 to 40, 4° effect, Roberts 3 to 12 2106 3" effect, : < Roberts 2to 12 - : -39- Basic procedures for entralament ‘monitoring ‘Types of entralament ‘Vapor velocities fn entrainmentIn South Affica, investigations at factories have shown that entrainment occurs through two main types of processes. Firstly, the sucrose loss correlates well with vapour velocity, through relationships of the form mg sucrose lost per unit time = a.(vapour velocity)” There are however, high, sporadic, losses which do not correlate with vapour velocity. This is illustrated in the following figure, for a centrifugal separator in a 2% effect, Roberts evaporator ENTRAINER (mais) 8838 8 SUCROSE ENTRAINE| 10 6 a VAPOUR VELOCITY (mis) Excluding the outliers, the relationship is 'mg sucrose lost / s = 19,1(vapour velocity)” for 20 pairs of observations with a correlation coefficient of 0,80. The sucrose lost through this entrainment process would be only about 50kg per week It can be seen however that, sporadic and high levels of sugar Contaminations were found, as shown by the squares in the figure. Very similar results were found with an angle iron separator in a 3“ effect, and with a centrifugal separator in a 4* effect -40- ‘Two pe of entrainment ‘processesSome concentrations of sugar in South Afritan condensates are shown below. 10-25 - 10-30 steady operation 90 - 300 unsteady operation 200 - 300 unsteady operation 3.10.3 Some practical points Blocked separator return lines are often the cause of poor separator performance. In situ separator washing systems pave been described in the literature (Taylor, 1987; Lionnet, 1984). Sight glasses on external lines allow quick, visual assessments of performance, If no flow is evident, then the separator needs investigation. Finally, a steady vacuumis a prerequisite for controlling entrainment. -41- Concentrations of sgn in ‘condensatesBIBLIOGRAPHY Austemeyer KE, Morgenroth B and Mauch W (1995). Plate evaporators in the sugar industry. Proc Int Soc Sug Cane Technol, 22" Conf: 91-102 Bhagat JJ (1995). 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Walthew DC, Whitelaw RW and Peacock SD (1995). Preliminary results from a long tube climbing film pilot evaporator. Proc § Afr Sug Technol Assoc 69: 132-137 Walthew DC, Morgenroth B, Diringer T, Hattwig N, Preybylak P and Friedrich C (1996), Pilot Plant investigations into a Balcke Darr falling film plate evaporator at GH sugar factory. Proc S Aft Sug Technol Assoc 70: 226-232, Walthew DC and Whitelaw RW (1996), Factors affecting the performance of long tube ‘climbing film evaporators. Proc S Afr Sug Technol Assoc 70: 221-224, Walthew DC, Whitelaw R and Mohabir R (1997). Chemical cleaning of evaporators. Proc S Afr Sug Technol Assoc 71: 199-206 Walthew DC, Wienese A, Squires R and Friedrich C (1996), Preliminary assessment of arising film plate evaporator. Proc $ Aff Sug Technol Assoc 70: 225-230, Walthew DC and Turner LM (1995). Analysis of scale from some South Aftican sugar mills. Proc S Aff Sug Technol Assoc 69: 138-143, Watson LJ (1987). Heat transfer mechanisms in evaporators. Proc Aust Soc Sug Cane Technol Assoc: 221-227. Webb BL and Koster KC (1991). A review of energy management and improvements at Noodsbergsugar mill over the past eight years, Proc $ Afr Sug Technol Assoc 65: 202-204. Wong Sak Hoi L and Tse Chi Shum S (1996). Estimation of sucrose inversion in evaporators. Proc S Afr Sug Technol Assoc 70: 236-240.SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS 1 Clarification 2 Filtration 3 Chemistry of cane and juices 4 Chemical control 5 Evaporation. The fundamentals 6 Evaporation, The practice In preparation:- Diffusion Crystallisation Pan boiling Carbonatation (refining) Sulphitation (refining) Phosphatation (refining)