Clarification Mixed juice extracted from the cane by milling or diffusion contains many impurities.

These are present as: i) Insoluble matter ii) Colloidal matter iii) Soluble species Purpose of clarificationTo produce a clear juice that is: i) of correct pH value,

ii) free of suspended or colloidal matter and to do this with minimum loss of sucrose or destruction of reducing sugars. Effect of clarification on quality of sugarClarification represents perhaps the only opportunity a process manager has of improving or modifying the cane juice. Hence, efficiency of clarification will have an important bearing on the quality of the sugar produced. Major constituents of cane juice

In solution
1. Sucrose 2. Reducing sugars Removal: By the action of heat, under alkaline conditions. Products will be highly coloured. Degradation of reducing sugars must be prevented. 3. Inorganic salts ( or ash) They are K, Na, Ca, Mg and Fe salts. Silicate, Sulphates, Chlorides & inorganic phosphate are also present. 4. Organic salts

In suspension
1. Bagasse 2. Sand 3. Clay 4. Chlorophyll Chlorophyll and other plant pigments are removed / destroyed during clarification 5. Wax Originated from nodes in the rind. Removal: Is physically removed with muds during clarification. It can be recovered from the filter cake

5. Organic acids e.g oxalic tannic, citric, tartaric acid. Impacts of oxalic acid: 1) They will form soluble lime salts and are not removed by clarification. 2) will form calcium oxalate which will precipitate at higher brixes in the last vessels of evaporators, forming hard scale 6. Pectins These are gelatinous carbohydrates in colloidal form Impacts: They increase viscosity Removal: They are precipitated during clarification, thus removed. 7. Gums These are colloidal polysaccharides. Impacts: They cause severe viscosity problems later in the process. Removal: They might/might not be removed during clarification 8. Protein They originate from cane tops and trash Removal: They are removed by heat and lime during clarification. 9. Colour bodies e.g saccaretin found in fibre, and chlorophyll, authocyanins, and polyphenols impacts: Acted upon by enzymes, by chemical oxidation and reaction with Fe, they will form dark-coloured soluble compounds. Removal: Chlorophyll and other plant pigments are removed / destroyed during clarification 10.Tannins and finally 11. Iron

6. Starch Is present as granules in the juice but they are soluble above 700. Removal: When soluble, it is not removed by clarification However it can be removed by thermally stable starch degrading enzyme, alphaamylase. Alpha-amylase is usually added at the evaporation stage. Impacts: Soluble starch gets incorporated into the raw sugar crystal Will cause filtration problems during refining. 7. Air Impacts: Air will interfere in any clarification process involving settling. Removal: Must be removed before sedimentation/settling of solids takes place

compounds Defecation/ Decantation Universally used agents for cane juice clarification are lime and heat. Defecation process is the universal process used in South Africa for clarification. It is a process comprising of major steps: 1. heating, 2. liming, 3. flashing and 4. settling.

1. HEATING Heat causes coagulation of some organic constituents. Eg. Proteins It increases the rate of rxn between lime and juice acids. Usually this rate is very slow at low Temp. Heating above b.p can cause flashing, thus air being removed. Heat also destroys micro-organisms and enzymes, thus preventing losses of sucrose by microbiological activity.

2. LIMING* It changes the pH of juice from slightly acidic to neutral/ alkaline pH. This reduces inversion and alkaline degradation of reducing sugars. It causes coagulation of some colloids. Insoluble lime salts, coagulated albumin and varying proportions of fats, waxes and gums form a very complex and heavy precipitate- the ppt formed will depend on type and maturity of cane, clarification procedure & pH NOTE: if inorganic phosphate level is <300ppm, juice cannot be clarified properly. Phosphate can be added in the form of phosphoric acid, phosphoric acid paste & mono-calcium phosphate. Phosphate in the juice is measured as P2O5.

The flocculated precipitate carries with it most of the finely suspended material left in the juice.

3. FLASHING Before flashing , juice should be heated to 1030C Flashing removes/ force out air from the juice and floc, to cause bagacillo to burst and sink with solids. It also results in uniform, constant Temp. of the limed juice, preventing thermal currents, promoting settling We must be observing condensed vapour being given off the flash-tank vent pipe. The vent pipe must be designed to obtain upward velocity of 1.7 ms-1 We must ensure that juice leaves the flash tank at approx. 1050C Diameter of flashtank will depend on juice downward velocity of juice for effective bubble escape

4. SETTLING Settling allows the precipitate to flocculate and collect at bottom of the vessel. In short retention type clarifier, flocculation and settling are helped by the addition of synthetic water soluble polymers. Good flocculatants will imporove flocculation, settling rate, mud volume, pol in cake and will increase clarity of clarified juice Performance of the polymers is affected by time of agitation of stock solution. Solvent ionic strength , polymer concentration, pH change due to addition of phosphate, concentration of calcium in the clear juice Settling rate is influenced by 1. Particle and liquid density, 2. Shape and diameter of particles, 3. Viscosity of liquid. Only shape and size of particles can be controlled At bottom of the vessel, compaction of the precipitate takes place. Clear juice can be removed from the top of the vessel

Note: -

Good juice flow control is vital for proper clarification.

Large and sudden variation in juice flow interferes with heating and liming + physically disrupts the contents of the clarifiers. Therefore, the floc contaminates the clear juice.

*South African practice: The simple lime defecation Mixed juice is generally dark & slightly acidic (pH 5.2- 5.8). In order to obtain clear light-colored juice: it is heated to boiling point, followed by addition of milk of lime. Neutralization reaction between lime and juice (juice acids) is controlled so as to obtain a clear juice of pH 7.0-7.2. The temperature is raised to maximum of 103-105 0C but shouldnt drop below b.p Juice is then flashed to atmosphere. After heating and liming, the limed-juice is sent to decant in large vessels called clarifiers. Juice will separate from precipitated solids. The juice is removed from the top (overflow) . the solids are removed from the bottom ( underflow)

Lime and Milk of Lime Lime = CaO Lime preparation: i) By burning limestone CaCO3 and coke in kilns. This method is used in the case of back-end refineries ( Pongola, Gledhow and Malelane ) the following reactions take place C + O2 = CO2 + heat CaCO3 + heat = CaO +CO2 Advantage: The CO2 generated can be used for the carbonatation process in refining. ii) Obtained from suppliers as lumps. Storage: CaO has high affinity for moisture and CO2 from atmosphere. Therefore it should be kept in low stocks in a protected environment. In modern installations, lime lumps are stored in closed bins

Use of lime in clarification process Lime is never added to the juice as CaO because of its action on reducing sugars. It is added to juice in the form of: i) Lime-saccharate Is soluble does not settle in pipes and tanks. ii) Milk of lime Will tend to deposit in pipes and tanks. It must be stirred and circulated to prevent settling

Therefore milk velocity in pipes must be 1ms-1

Can be left standing during weekend shut-down & be immediately available at start-up Produces clear juice of higher turbidity

Will producse clear juice with lower turbidity than milk of lime does

Will tend to produce lighter & more voluminous muds

Lime saccharate

Milk of Lime

Is used in few factories only. Preparation:

Milk of lime has only one important property for clarification: its neutralizing capacity The lime undergoes the slaking process to produce milk of lime or Calcium Hydroxide/ slaked lime . The reaction is exothermic. CaO + H20 = Ca (OH)2 + 63.61kJ Calcium oxide Calcium Hydroxide/ slaked lime is only sparingly soluble in water (1 part/ 790 part of H20)

Reaction between milk of lime and sugar solutions, depending on the chemical and physical conditions under which it takes place, gives rise to possible formation of mono, di and tri-calcium saccharates. But the objective is to obtain mono-saccharate which is most soluble. Conditions to be maintained to ensure formation of highly soluble monosaccharates: a) Sucrose in excess In practice the required ration of sucrose to calcium is 7:1. This ratio is obtained by using evaporator syrup (680brix) on 150 Beaume milk of lime. Resulting pH of saccharate solution is 11.0-11.15. Thus we ensure excess sucrose and control the saccharate formation at pH 11.0 in order to assure mono-calcium saccharate formation b) Temp. < 58oC Equn for formation of mono-calcium saccharate: C12H22O11 + Ca (OH)2 = C12H20O11Ca + H20

Ca (OH)2 is present as a fine suspension of small particles in water. This slaked lime/ Calcium Hydroxide / Ca (OH)2 is applied to the juice in about 8o beaume. In cabonatation refineries it is prepared between 12-15 beaume using clean, hot condensate.

Quality of lime is of prime importance in clarification. There should be approx 85 % of CaO available

Different Heating and Liming Techniques1. Cold liming / lime-heat method Cold liming got pH of 7.5- 8.2, followed by heating to 100-102oC. Disadvantage: bacterial activity problem 2. Lime- heat- lime heat/ Fractional liming ( no application nowadays) Cold Liming to pH 6.5, heating to 90oC, followed by liming to pH 7.5-8.2 and heating to b.p Disadvantage: liming twice is a difficulty 3. Liming at 700C and heating to b.p ( no application nowadays) 4. Hot liming ( universally used nowadays) Juice is limed before flashing Juice is heated and reaches flash tank at 1020C-1050C pH is controlled during all the process Advantages of hot liming: 1) Effective precipitation is possible at low pH 2) Less time consuming 3) More rapid settling Disadvantage: 1) Sucrose Inversion risk are higher 2) Muds are lighter and more voluminous

Effect of pH 1. Rate of sucrose inversion increases as pH lowers ( becomes more acidic ) and temperature increases 2. Hight pH and high temperatures destroy reducing sugars

3. Inversion and degradation rates depend on retention time which cannot be control so we control pH To undertake pH control: we minimize fluctuation in juice flow and lime concentrations by providind sufficient buffer capacity in juice stream and lime preparation stage before lime addition.

Clarifiers Serve to separate juice from floc Two types are: Dorr and Trayless