US3926662A - Production of cane sugar - Google Patents

Abstract

A process for removing suspended solid impurities from sugar cane evaporated juice or sugar cane affination syrup comprises adding a soluble phosphate salt to said sugar to form therein an insoluble calcium phosphate primary floc containing said suspended impurities, aerating the liquor containing the primary floc, with agitation, distributing uniformly throughout the aerated liquor from 1-40 parts by weight of an anionic flocculating agent per million parts by weight of sugar in the liquor to initiate the formation of a secondary floc therein, said flocculating agent being a polymer with a molecular weight from 1,000,000 to 10,000,000 containing 50-80 mol percent acrylamide units and from 50-20 mol percent of anionic units, retaining the resulting mixture for from 15 seconds to 5 minutes in a flocculator vessel with non-turbulent agitation preventing the segregation of the secondary floc from the liquor and allowing the secondary floc to grow, transferring the liquor containing the secondary floc with minimal agitation and shear from the flocculator vessel to a separator vessel, allowing the secondary floc to segregate by flotation from the liquor in the separator vessel, and separately removing clarified liquor and flocculated solids from the separator vessel.

Description

[ Dec. 16, 1975 1 PRODUCTION OF CANE SUGAR [75] Inventors: John Trethowan Rundell, Keston;

Paul Richmond Pottage, Bromley, both of England [73] Assignee: Tate & Lyle Limited, London,

England [22] Filed: Sept. 23, 1974 [21] Appl. No.: 508,195

Related US. Application Data [63] Continuation-impart of Ser. No. 263,784, June 19,

1972, Pat. No. 3,853,616.

[30] Foreign Application Priority Data Sept. 28, 1973 United Kingdom 45516/73 [52] U.S. Cl. 127/48; 127/50, 127/57;

[51] Int. Cl. C131) 3/00 [58] Field Of Search 127/48, 50, 57

[56] References Cited UNITED STATES PATENTS 1,317,607 9/1919 Williamson 127/57 3,098,766 7/1963 Payet 127/48 X 3,166,442 l/1965 Duke 127/48 3,508,965 4/1970 Harrison 127/48 3,698,951 10/1972 Bennett 127/48 3,853,616 12/1974 Rundell 127/48 Primary ExaminerMorris O. Wolk Assistant ExaminerSidney Marantz Attorney, Agent, or Firm-Ostrolenk, Faber, Gerb & Soffen [5 7] ABSTRACT A process for removing suspended solid impurities from sugar cane evaporated juice or sugar cane affination syrup comprises adding a soluble phosphate salt to said sugar to form therein an insoluble calcium phosphate primary floc containing said suspended impurities, aerating the liquor containing the primary floc, with agitation, distributing uniformly throughout the aerated liquor from 1-40 parts by weight of an anionic flocculating agent per million parts by weight of sugar in the liquor to initiate the formation of a secondary floc therein, said flocculating agent being a polymer with a molecular weight from 1,000,000 to 10,000,000 containing 50-80 mol percent acrylamide units and from 50-20 mol percent of anionic units, retaining the resulting mixture for from 15 seconds to 5 minutes in a flocculator vessel with non-turbulent agitation preventing the segregation of the secondary floc from the liquor and allowing the secondary Hoe to grow, transferring the liquor containing the secondary floc with minimal agitation and shear from the flocculator vessel to a separator vessel, allowing the secondary floc to segregate by flotation from the liquor in the separator vessel, and separately removing clarified liquor and flocculated solids from the separator vessel.

10 Claims, 1 Drawing Figure US. Patent Dec. 16, 1975 3,926,662

PRODUCTION OF CANE SUGAR This application is a continuation-in-part of application Ser. No. 263,784, filed June 19, 1972, and now US. Pat. No. 3,853,616.

BACKGROUND OF THE INVENTION This invention relates to improvements in the production of cane sugar.

The production of cane sugar for human consumption generally comprises two distinct operations, namely the production of raw sugar and the production of refined sugar, which are often carried out in geographically separate locations. In the manufacture of raw sugar, the raw juice obtained from sugar cane is normally subjected to deaeration in a flash tank, clarifiction (i.e., removal of suspended solids by sedimentation), evaporation to a thick syrup (known as evaporated juice) in a multiple-effect vacuum evaporator, and crystallization in a vacuum pan. The massecuite (i.e., mixture of sugar syrup and crystals) produced in the vacuum pan is slowly stirred in a so-called crystallizer, and the mother syrup is then spun off from the raw sugar crystals in a centrifugal separator. In order to remove the film of syrup clinging to the surface of the sugar crystals, the wall of solid sugar in the centrifugal basket is washed with water inevitably, some of the sugar is redissolved, and the resulting solution is returned to process for recovery of the sugar. If special processing is introduced into these stages, the crystallized product can reach a standard suitable for direct consumption, and is then known as Mill White or Plantation White sugar; but generally raw sugar must be refined before it reaches an acceptable standard of purity.

In the conventional cane sugar refining process, the raw sugar is first washed and centrifuged to remove adherent syrup, and the affined sugar thus produced is dissolved in water as melter liquor. The syrup removed from the surface of raw sugar is known as affination syrup and is broadly similar in composition to evaporated juice. It is treated in the recovery house of the refinery, where it passes through vacuum pans, crystallizers" and centrifugal separators similar to those used for the production of raw sugar, to recover an impure crystalline sugar product which has approximately the same composition as raw sugar. This recovered sugar product is dissolved in water, along with the affined raw sugar, to make melter liquor. Thus, the treatment of affination syrup in the recovery house of the refinery can broadly be equated with the production of raw sugar from evaporated juice.

The melter liquor is then purified, generally by the successive steps of defecation" and decolorization, and the resulting fine liquor is crystallized to give refined sugar although the decolorization step may be omitted altogether when a relatively low quality refined sugar product is required. The defecation step most frequently involves forming an inorganic precipitate in the liquor, and when this precipitate is removed it carries along with it insoluble and colloidal impurities which were present in the melter liquor. In one of the defecation processes commonly used for melter liquor, termed phosphatation, the inorganic precipitate is calcium phosphate, normally formed by the addition of lime and phosphoric acid to the liquor. The calcium phosphate precipitate is usually removed from the liquor by flotation, in association with air bubbles.

Many chemical additives have been recommended to aid the flotation separation of suspended solids from aqueous liquors, including high. molecular weight anionic polymeric flocculating agents of the polyacrylamide type. However, it is found that the mere addition of such flocculants will not necessarily give rise to the efficient flocculation which is needed in order to achieve subsequent rapid and complete clarification of the liquor. In particular, as described and claimed in our copending application Ser. No. 263,784, we have previously discovered that optimum flocculation of the suspended solids and efficient clarification of the liquor can be achieved by a process which comprises: forming a primary floc in the liquor containing suspended solids; aerating the primary floc, with agitation; distributing an organic polymeric flocculant uniformly throughout the liquid phase of the aerated liquor, to initiate the formation of a secondary floc therein; retaining the resulting mixture in a flocculator vessel with non-turbulent agitation preventing the segregation of the secondary floc from the liquor and allowing the secondary floc to grow; transferring the liquor, with minimal agitation, from the flocculator vessel to a separator vessel; allowing the secondary floc to segregate by flotation from the liquor in the separator vessel; and separately removing clarified liquor and flocculated solids from the separator vessel. Our US. Pat. No. 3,834,541 describes and claims an apparatus which allows this improved flotation process to be carried out in a particularly advantageous way.

The improved process of our copending application Ser. No. 263,784 is described in detail therein with particular reference to the defecation of cane sugar melter liquor by phosphatation/flotation, although it is applicable to the removal by flotation of suspended solids from aqueous liquors in general, including sugar juices, liquors and syrups found in various stages of cane and beet sugar manufacture. However, it has now been discovered that certain modifications of and departures from the preferred manner of operating the process for the purification of melter liquor enable it to be applied more advantageously to the purification of evaporated juice and affination syrup.

The terms evaporated juice, thick juice, thick syrup and meladura are all used by sugar manufactures to describe the same material, i.e.., a concentrated sugar solution which has been obtained by the evaporation of a sugar juice. For the avoidance of confusion,

only the term evaporated juice will be used in relation to the present invention. It will be understood that this term means juice which has undergone at least one stage of evaporation, thus, in the case of a multipleeffect evaporator train, the evaporated juice can be that taken from one of the intermediate effects, as well as that obtained from the last effect of the evaporator and from which raw sugar is eventually crystallized.

Evaporated juice and affination syrup are very similar to each other but differ significantly from melter liquor in their composition, particularly in their much higher impurity content. Thus, whereas crystalline raw cane sugar typically has a sucrose content greater than 95% by weight, and melter liquor has a sucrose content of about 99% by weight on solids, the typical sucrose contents of evaporated juice and affination syrup are, respectively, about and about by weight on solids. Evaporated juice and affination syrup have a much higher turbidity than melter liquor, being almost opaque; they contain suspended matter, such as soil and cane-fibre particles, which are never completely removed during the clarification step, and also precipitated inorganic salts and flakes of scale which are deposited during the evaporation. They also have a relatively high content of dissolved impurities, and in particular typically have a calcium ion concentration of about 2,000 ppm. In the conventional process of raw sugar manufacture, there is no provision for removing dissolved or suspended impurities from the evaporated juice before the crystallization of the raw sugar; and similarly, in the conventional refining process, there is noprovision for removing such impurities from the affination syrup before it is passed to the pans in the recovery house. The present invention provides an effective process for the removal of such impurities at these stages, and it has been found that this leads to considerable advantages in the subsequent processing of the sugar.

SUMMARY OF THE INVENTION The invention provides a process for removing suspended solid impurities from a sugar liquor which is cane sugar evaporated juice or affination syrup, which comprises: adding a soluble phosphate salt to said sugar liquor, to form an insoluble calcium phosphate primary floc containing said suspended impurities; aerating the liquor containing the primary floc, with agitation; distributing uniformly throughout the aerated liquor from I to 40 parts by weight of anionic flocculating agent per million parts by weight of sugar in the liquor, to initiate the formation of a secondary floc therein, said flocculating agent being a polymer with a molecular weight of from 1 million to million containing from 50 to 80 mole percent of acrylamide units and from 50 to 20 mole percent of acrylic acid and/or acrylate units; retaining the resulting mixture for from seconds to 5 minutes in a fiocculator vessel with non-turbulent agitation preventing the segregation of the secondary floc from the liquor and allowing the secondary floc to grow; transferring the liquor containing the secondary floc with minimal agitation and shear from the flocculator vessel to a separator vessel; allowing the secondary floc to segregate by flotation from-the liquor in the separator vessel; and separately removing clarified liquor and flocculated solids from the separator vessel.

The process of the invention performs a number of functions which result in substantial advantages during the subsequent processing of the sugar. It results in the removal of insoluble suspended solids which have been carried over during the clarification of the juice. especially juice, particles which are found more frequently with the increasing use of mechanical harvesting of the sugar cane, and also inorganic insoluble salts which have been precipiated during the evaporation stage and some of which form scale that can subsequently flake off. It also results in the removal of calcium ions which would otherwise also form insoluble scale (either in the last effect of the evaporator or on the calandria of the vacuum pan) and which, in association with high molecular weight acidic polysaccharide impurities in the evaporated juice or affination syrup, would otherwise cause a substantial increase in both structural and Newtonian viscosity. The removal of particulate impurities from the evaporated juice or affination syrup facilitates the subsequent centrifugal separation of the mother syrup from the sugar crystals, by avoiding clogging of the interstitial spaces in the wall of sugar crystals which forms in the centrifugal basket, so. that less water is 4 needed to wash the syrup from the crystals and consequently less sugar is redissolved. The removal of particulate impurities which would otherwise be occluded in the sugar crystals also leads to a product of lower turbidity, which appears brighter and less coloured, this improved product, whether a raw or recovered sugar,

has an enhanced value because it needs less refining to bring it to an acceptable standard for human consumption. The lowering of the viscosity, resulting from the reduction of the calcium ion concentration, leads to easier stirringin the crystallizers, allowing greater crystallization of sucrose before the centrifugal separation step. It also results in better circulation of the massecuite in the vacuum pan, which reduces the incidence of false grain generation and thereby produces a more uniform crystal product. This, in turn, facilitates the centrifugal separation of the mother syrup from the crystals, in the same way as does the removal of particulate impurities, so that less water is needed to wash the sugar crystals and less sugar is redissolved. The incidence of false grain generation'is also reduced by the removal of insoluble particles such as fragments of cane fibre.

DETAILED DESCRIPTION OF THE INVENTION Evaporated juice taken from the last effect of a multiple-effect evaportor typically has a sugar concentration of 65 Brix and a temperature of about C. Affination syrup typically has a sugar concentration of -75 Brix, and is preferably diluted to about 60 Brix before being subjected to the process of the invention. The optimum temperature for the process of the invention is -85C, and it is generally necessary to heat the evaporated juice or affination syrup in order to raise its temperature to this level, suitably by passing it through a heat exchanger; this can be done either at the very beginning of the process or after the formation of the primary floc.

In the first stage of the process of the invention, a primary floc is formed by adding a soluble phosphate salt to the evaporated juice or affination syrup. It is possible to use a soluble calcium salt, such as monobasic calcium phosphate or triple superphosphate, but it is preferred to use a non-calcium salt, such as Na P0 Na I-IPO or NaI-I PO so as to obtain the full advantage of reducing the calcium ion concentration in the juice or syrup. The phosphate is conveniently added in the form of an aqueous solution having a concentration of about 10% by weight. It is generally added at a level corresponding to -600, preferably 200400, parts per million by weight of P 0 on the basis of the sugar in the juice or syrup. The phosphate reacts with the calcium ions present in the juice or syrup, forming a fiocculent precipitate of insoluble calcium phosphate. This precipitate entrains suspended impurities and also adsorbs high molecular weight dissolved impurities from the juice or syrup. Since the calcium phosphate precipitation reaction occurs quite slowly, it is preferred to add the phosphate to the juice or syrup' in a suitable vessel, such as a stirred tank, where it can be retained with mixing for about 2 minutes, to allow completion of the precipitation.

The use of a soluble phosphate salt, such as a sodium orthophosphate, for the formation of the primary floc, as opposed to the use of lime and phosphoric acid in the conventional phosphatation treatment, provides important practical advantages. When lime is used, its addition must be very carefully balanced against that of phosphoric acid, to keep the pH within acceptable limits. By using a salt such as a sodium orthophosphate, only one reagent is added instead of two, no pH control is required, and also the concentration of calcium in the juice is reduced. These factors render the process of the invention substantially more economical and efficient.

If the temperature of the evaporated juice or affination syrup is not already in the range of 7585C, it is desirable to bring it within this range after the formation of the primary floc, suitably by passing the juice or syrup through a heat exchanger. The juice containing the primary floc is then aerated. The injection of air is essential, because evaporated juice has been efficiently deaerated in the flash tank prior to the clarification step and then in the evaporator itself, and affinated syrup also needs additional aeration. Efficient aeration can be achieved, for example, by the injection of air into the juice or syrup which is passed through a centrifugal pump with an impeller operating at a tip speed of about 30 meters per second. Alternatively, a highspeed high-shear aerator can be used, operating with a rotor speed of about 3,500 rpm. Satisfactory results can be obtained with an aerator capable of supplying about one-half horsepower per ton per hour of solids throughput. More efficient aeration can also be achieved by causing the juice or syrup to flow through 6 the one hand, good distribution of the flocculant cannot be achieved by merely dosing it into a volume of the juice or syrup; whilst, on the other hand, violent blending, such as produced in some in-line mixers or by passing the juice or syrup through a centrifugal pump, is also unsatisfactory. Thus, although good distribution is desirable, it has been found that completely homogeneous blending is undesirable. It is theorized that with too thorough mixing the flocculant molecules are lost within the growing flocs and can no longer gather together suspended solid particles to form larger flocs. The degree of distribution of flocculant molecules in the mixture will depend on the intensity and duration of mixing. For instance, the right degree of distribution is achieved by a degree of turbulence corresponding to Reynolds numbers from 3,000 20,000, preferably 5,000 to 10,000, for about 1 second. In practice, this satisfactory distribution can be achieved by dosing the flocculant through a metering pump into the aerated juice or syrup flowing with a linear velocity of from 0.3

a tank fitted with an external closed loop which includes the aerator, and arranging the rates 'of flow so that the juice or syrup passes several times through the aeration loop during its residence time in the tank.

The aerated juice or syrup is next dosed with an anionic acrylamide copolymer flocculating agent having a molecular weight of from 1 million to 10 million, preferably from 4 million to 8 million, containing from 50 to 80 mole percent of acrylamide units and from 20 to 50 mole percent of anionic units (i.e., acrylic acid and/or acrylate units). A suitable flocculating agent is that available under the Trade Mark TALODURA from Tate & Lyle Limited. The flocculating agent used in the process of the present invention differs from the preferred anionic acrylamide copolymer flocculating agent used for the treatment of melter liquor in the process of our aforementioned application Ser. No. 263,784, which contains only up to 20 mole percent of acrylic acid and/or acrylate units. From 1 to 40, preferably from 1 to 20 and most preferably 5 to 15, parts by weight of the flocculating agent are used per million parts by weight of sugar in the juice or syrup.

The manner in which the flocculant is added to the aerated juice or syrup can significantly affect the success of the subsequent steps. Thus, the flocculant should desirably be used in the form of a dilute aqueous solution, generally having a concentration of 0.025% to 0.5% w/v, preferably 0.05% to 0.2% w/v, since a greater dilution of the polymer molecules allows better utilization of the full activity of the flocculant. The flocculant solution should not be subjected to vigorous mechanical treatment, such as high speed agitation, which can rupture the polymer molecules; instead, an air stream can be used to dissolve the polymer. The flocculant solution should be aged for a few hours before use, to aid dissolution, but should not be kept longer than about one day otherwise hydrolysis and fragmentation of the polymer molecules can occur; generally, aging for 2 to 3 hours is satisfactory.

The satisfactory distribution of the polymeric flocculant in the aerated juice or syrup is also important. On

to 3 meters per second, preferably about 1.5 meters per second, in a pipe of appropriate bore; but the right degree of distribution can' also be obtained in other ways, such as by causing the juice or syrup to flow through a pipe containing one or two right-angle bends in it.

An alternative method of achieving the right degree of distribution of the flocculant in the juice or syrup involves pre-mixing the flocculant solution with a small fraction, say 2l0%, of the clarified juice or syrup being produced by the process of the invention. Because the clarified juice or syrup does not contain growing flocs, it can be subjected to more vigorous mixing than the untreated juice or syrup, for example using an in-line flow mixer. The pre-mix is then added to the untreated juice or syrup and distributed through it by gentle mixing. This procedure has the advantage that the flocculant can be used at high dilutions without having to add large quantities of water to the process 40 juice or syrup.

The mixture of the aerated juice or syrup and polymeric flocculant is then retained for a period of time in a flocculator vessel, under conditions of reduced linear velocity. In the flocculator vessel, the eddy currents and shearing forces imposed on the juice or syrup during its mixing withthe flocculant are allowed to die down, but a gentle non-turbuient agitation is maintained so as to prevent the segregation of the secondary flocs. This can be provided by a slowly rotating stirrer, for example, having a tip speed of from 0.3 to 1.5 meters per second, or by causing the juice or syrup to flow through a series of perforated static baffles. It has been found that the flocculation is greatly improved by retaining the floc within the body of the juice or syrup for a short period of time under quiescent conditions, before allowing it to separate out. It is thought that this retention time is needed for the flocculant molecules to become fully loaded with solid particles, and thus achieve the maximum degree of flocculation. Reten' tion times of from 15 seconds to 5 minutes are generally satisfactory, and times from 30 seconds to 3 minutes are preferred.

7 the flocs of solid material are allowed to separate out from the liquid, and the flocculated solids and clarified juice or syrup are removed separately, The flocs float to the top. and the clarified juice, or syrup is removed from the bottom. The separator vessel can be a conventional clarifier of one of the many known designs, with a flocculator vessel of suitable capacity connected in its influent feed, so as to provide the desired residence time for the juice or syrup. However, the retention and separation steps are preferably performed in an apparatus which combines the flocculator and separator vessels as separate chambers within the body of a single clarifier. Such an apparatus is described and claimed in our US. Pat. No. 3,834,541, and comprises: a separator chamber; a flocculator chamber centrally located within the separator chamber; a trough surrounding the top of the separator chamber; liquid inlet means located at the bottom of the flocculator. chamber; liquid agitating means located within the flocculator chamber; means allowing floc-containing liquid to flow with minimal agitation from the top of the flocculator chamber into the separator chamber; means for transferring floating flocculated solids from the top of the separator chamber to the trough; solids outlet means located at the bottom of the trough; and outlet means for clarified liquid located at the bottom of the separator chamber.

The invention will be further described with reference to the accompanying drawing, which shows a flow diagram for a process in accordance with the invention.

Referring to the drawing, evaporated juice or affination syrup is fed from the pipe 1 into the mixing tank 2, which is provided with stirrer 3 driven by motor 4. In the mixing tank, the juice is dosed through the pipe 5 with an aqueous solution of a soluble phosphate salt, which is supplied from holding tank 6 by means of the metering pump 7.

Typically after a residence time of about 2 minutes, the juice or syrup containing the calcium phosphate primary floc. leaves the holding tank 2 and passes through the heat exchanger 8 wherein it is heated by means of steam to a temperature of 7585C. (This step is not necessary if the evaporated juice or affination syrup is already at this temperature). The juice or syrup containing the primary floc is then aerated with agitation, by passing through the aerator 9 which is fed with compressed air from the line 10. Next, the aerated juice or syrup is dosed via pipe 11 with an aqueous solution of the anionic polymeric flocculating agent, which is supplied from holding tank 12 by means of the metering pump 13, to initiate the formation of secondary flocs therein. The juice or syrup then flows through a section of pipe 14 having right-angled bends in it, so as to provide the correct degree of turbulence in the mixture for uniform distribution of the flocculating agent.

The resulting mixture flows from the pipe 14 into the central flocculator chamber 15 of a clarifier of the type described in our US. Pat. No. 3,834,541. As it rises in the flocculator chamber 15, it is kept gently stirred by and surrounding annular sleeve 19, which direct the mixture to flow with minimal agitation and shear into the body of the separator chamber 20. In the separator chamber, the flocs rise to the top of the liquid as a scum, which is pushed into the annular trough 21 sur rounding the top of the chamber by means of the slowly rator'chamber via the multiple liquid outlets 24 which feed intothe pipe 25. In the case of clarified evaporated juice, it is either passed to the raw sugar vacuum pans or returned to the evaporator, depending upon whether the feed 1 to the process was taken from the last stage or an intermediate stage of the evaporator train; whilst in the case of clarified affination syrup, it is passed to the pans in the recovery house of the refinery.

The invention is illustrated by the following Examples.

EXAMPLE 1 This Example illustrates the effect on the efficiency of secondary floc separation of using acrylamide/acrylate copolymer flocculating agents with different degrees of anionic character.

The process described hereinbefore with reference to the accompanying drawing was used for the purification of a cane sugar evaporated juice from a Venezuelan raw sugar factory. The juice, having a concentration of 50 Brix and a temperature of 65C, was dosed with a 10% by weight aqueous solution of anhydrous trisodium orthophosphate at a level corresponding to 400 ppm of P on the basis of sugar solids. After a retention time of about 2 minutes in the mixing tank, the treated juice was heated to about 80C in the heat exchanger and then aerated by passage through a centrifugal pump with an open impeller. The aerated juice was dosed with ppm, on the basis of sugar solids, of an acrylamide/acrylate copolymer flocculating agent having a molecular weight of about six million, used in the form of a 0.1% w/v aqueous solution. The time taken for flocs to appear in the juice after entering the clarifier was taken as a measure of the efficiency of the process.

,The results obtained with flocculating agents of -60% anionic character are shown in Table 1.

Table 1 Time required for Flocs to Appear (seconds) It will be'clearly seen from Table 1 that markedly superior results are obtained when using the flocculating agents containing 20-50 mole percent of acrylate units, in accordance with the present invention, than when using the flocculating agents having a composition outside these limits, shown here for comparative v purposes.

EXAMPLE 2 This Example shows the effect of juice temperature on the speed of the secondary flocculation.

The procedure of Example 1 was repeated, except that the aerated juice was dosed in each run with 8 ppm by weight (on the basis of sugar solids) of the flocculating agent having 40% anionic character, and the temperature of the juice entering the clarifier was varied in each run. The results obtained are shown in Table 2.

Table 2 Juice Temp. (C) Time required for Flocs to Appear (seconds) EXAMPLE 4 10 juice and decolorization with sodium hydrosulphite (in order to reach an acceptable standard of purity) prior to boiling in vacuum pans.

The conventional phosphatation process was replaced by the process of the invention, as described 2; hereinbefore with reference to the accompanying 75 4 drawing. The evaporated juice, having a concentration 85 3 of 60 Brix and a temperature of 80C, was dosed with a 10% by weight aqueous solution of trisodium orthophosphate, at a level corresponding to 497 ppm of It Wlil be seen that the time required for the secondp 0 b i h on h b i f Sugar hd Af flees to hh decreases ptegtesslvely as the pe aeration, the juice was dosed with 20 ppm by weight, ature of the Jutee 1s raised; but temperatures of 90 C on the basis of sugar solids, of the same flocculating and above should be avo ded, becaus 0f thermal gagent as used in Example 2. The mixture of juice and radatloh of sucrose, leadlhg to less of p secondary fioc was retained in the flocculator chamber f the clarifier for 2 minutes EXAMPLE 3 Table 4 shows the consumption of chemicals in the Thls Example illustrates the effect of e P ph old and new processes, and compares the quality of {dosage level Oh t turbldlty e the heated .l Whleh sugar produced by the two processes. The turbidity and 1s a measure of Its lhsohlhle hhphhtles eohtehtcolour were measured in terms of optical density at 420 The Procedure of Example 1 was repeated eep nm, in milliabsorbency units; and the ash content was that the p p te ge level was Varled, the l h measured conductimetrically, and is expressed in per- WaS heated t 75 and In a run the aerated lulee cent by weight. The results clearly demonstrate that the s dosed Wlth 10 Pp hy Weight t basls of s ga replacement of the conventional phosphatation process SOhdS) 0f the fleeeulatlhg ag having 9 ahlehle by the process of the invention. gives a markedly supecharacter. The results obtained are shown in Table 3, i product, at the Same time as permitting the use f the tutbldlt) of the treated Jlhee bethg measured In lower levels of phosphate and hydrosulphite.

Table 4 Quality of Plantation White" Process Consumption of chemicals Produced (ppm by weight on sugar Turbidity Colour Ash solids) (m.a.u.) (m.a.u.) (7c) Conventional Phosphoric acid 1640 phosphatation (calculated as P205, 1081 399 0.071 Sodium 4080 Hydrosulphite Process of Trisodium 497 invention phosphate (calculated as 2 5) Sodium 2680 268 269 0.046 Hydrosulphite Flocculant 20 terms of optical density at 420 nm, in milliabsorbency EXAMPLE 5 units.

Table 3 Phosphate dosage Turbidity (m.a.u.)

This Example illustrates the purification of affination syrup by the process of the invention.

The process as described hereinbefore with reference to the drawing was used for the purification of affination syrup from the Thames refinery of Tate & Lyle Limited, England. The syrup, having a concentration of 60 Brix and a temperature of C, was dosed with a 10% by weight aqueous solution of anhydrous trisodium orthophosphate, at a level corresponding to 500 ppm by weight of P 0 on the basis of sugar solids. The syrup containing calcium phosphate primary floc was aerated, then dosed with 20 ppm by weight, on the basis of sugar solids, of the same flocculating agent as used in Example 2. The syrup was then passed to the Table 5 Reduction Reduction Treatment Turbidity in Tur- Colour in (m.a.u.) bidity (72) (m.a.u.) Colour (7:)

None 15.320 26,940 Process of 4,220 72 24,300 10 invention 12,150

EXAMPLE 6 This Example illustrates the purification of evaporated juice by the process of the invention, in order to obtain a raw sugar product of superior quality. The parameter used for measuring the quality of the raw sugar in this Example is that of filterability. This is measured by filtering a solution of the raw sugar under controlled conditions, as specified in the CSR Filterability Test", as described at page 271 of the Proceedings of the lntemational Society of Sugar Cane Techriologists, Ninth Congress, 1956. Under the test conditions, a solution of granulated refined sugar would give a filterability value of 100%. Filterability is widely recognised by sugar refiners as a measure of the quality of raw sugar.

The process of the invention, as described hereinbefore with reference to the drawing, was used for the purification of a cane sugar evaporated juice from a South African raw sugar factory. The juice, having a concentration of 60 Brix and a temperature of 80C, was dosed with a 10% by weight aqueous solution of anhydrous trisodium orthophosphate, at a level corresponding to 300 ppm by weight of P on the basis of sugar solids. The juice containing calcium phosphate primary floc was aerated and then dosed with ppm by weight, on the basis of sugar solids, of the same flocculating agent as used in Example 2. The retention time in the flocculator chamber of the clarifier was 2 minutes.

Before installation of the process of the invention, the raw sugar produced in the factory had a filterability value of 45%. The average filterability value of the raw sugar produced over a period of 4 weeks, using the process of the invention for the purification of the evaporated juice, was 71%. This clearly demonstrates the substantial improvement in raw sugar quality obtained by using the process of the invention.

We claim:

1. In a process for removing suspended solid impurities from a calcium-containing sugar liquor selected from the group consisting of cane sugar evaporated juice and cane sugar affination syrup, which comprises: forming therein an insoluble calcium phosphate primary floc containing said suspended impurities; aerating the liquor containing the primary floc, with agitation; distributing uniformly throughout the aerated liquor from 1 to 40 parts by weight of anionic flocculating agent per million parts by weight of sugar in the liquor, to initiate the formation of a secondary floc therein, retaining the resulting mixture for from 15 seconds to 5 minutes in a flocculator vessel with nonturbulent agitation preventing the segregation of the secondary floc from the liquor and allowing the secondary floc to grow; transferring the liquor containing the secondary floc with minimal agitation and shear from the flocculator vessel to a separator vessel; allowing the secondary floc to segregate by flotation from the liquor in the separator vessel; and separately removing clarified liquor and flocculated solids from the separator vessel; the improvement which comprises forming said insoluble calcium phosphate primary floc by adding a soluble phosphate salt to said sugar liquor and employing as said anionic flocculating agent a polymer with a molecular weight of from one million to ten million containing from 50 to mole percent of acrylamide units and from 50 to 20 mole percent of anionic units selected from the group consisting of acrylic acid and acrylate units. i

2. A process according to claim 1, wherein said soluble phosphate salt is a sodium orthophosphate.

3. A process according to claim 1, wherein said soluble phosphate salt is added in an amount corresponding to from to 600 parts by weight of P 0 per million parts by weight of sugar in said liquor.

4. A process according to claim 3, wherein said soluble phosphate salt is added in an amount corresponding to from 200 to 400 parts by weight P 0 per million parts by weight of sugar in said liquor.

5. A process according to claim 1, wherein said flocculating agent has a molecular weight of from four million to eight million.

6. A process according to claim 1, wherein from 1 to 20 parts by weight of said flocculating agent are used per million parts by weight of sugar in said liquor.

' 7. A process according to claim 1, wherein said mixture is retained in said flocculator vessel for a period of from 30 seconds to 3 minutes.

8. A process according to claim 1 wherein said flocculating agent is an acrylamide/acrylate copolymer' having a molecular weight of about six million. v

9. A process according to claim 8 wherein said flocculating agent has 40% anionic units.

10. A process according to claim 1 wherein said soluble phosphate salt is a sodium orthophosphate and is added in an amount corresponding to from 200-400 parts by weight of P 0 per million parts by weight of sugar in said liquor, wherein said flocculating agent has a molecular weight of from four million to eight million and is employed in an amount from 1-20 parts by weight per million parts by weight of sugar in said liquor, and wherein said mixture is retained in said flocculator vessel for a period of from 30 seconds to 3 minutes.

Claims (10)

1. IN A PROCESS FOR REMOVING SUSPENDED SOLID IMPURITIES FROM A CALCIUM-CONTAINING SUGAR LIQUOR SELECTED FROM THE GROUP CONSISTING OF CANE SUGAR EVAPORATED JUICE AND CANE SUGAR AFFINATION SYRUP, WHICH COMPRISES: FORMING THEREIN AN INSOLUBLE CALCIUM PHOSPHATE PRIMARY FLOC CONTAINING SAID SUSPENDED IMPURITIES; AERATING THE LIQUOR CONTAINING THE PRIMARY FLOC, WITH AGITATION; DISTRIBUTING UNIFORMLY THROUGHOUT THE AERATED LIQUOR FROM 1 TO 40 PARTS BY WEIGHT OF ANIONIC FLOCCULATING AGENT PER MILLION PARTS BY WEIGHT OF SUGAR IN THE LIQUOR, TO INITIATE THE FORMATION OF A SECONDARY FLOC THEREIN, RETAINING THE RESULTING MIXTURE FOR FROM 15 SECONDS TO 5 MINUTES IN A FLOCCULATOR VESSEL WITH NON-TURBULENT AGITATION PREVENTING THE SEGREGATION OF THE SECONDARY FLOC FROM THE LIQUOR AND ALLOWING THE SECONDARY FLOC TO GROW; TRANSFERRING THE LIQUOR CONTAINING THE SECONDARY FLOC WITH MINIMAL AGITATION AND SHEAR FROM THE FLOCCULATOR VESSEL TO A SEPARATOR VESSEL; ALLOWING THE SECONDARY FLOC TO SEGREGATE BY FLOTATION FROM THE LIQUOR IN THE SEPARATION VESSEL; AND SEPARATELY REMOVING CLARIFIED LIQUOR AND FLOCCULATED SOLIDS FROM THE SEPARATOR VESSEL; THE IMPROVEMENT WHICH COMPRISES FORMING SAID INSOLUBLE CALCIUM PHOSPHATE PRIMARY FLOC BY ADDING A SOLUBLE PHOSPHATE SALT TO SAID SUGAR LIQUOR AND EMPLOYING AS SAID ANIONIC FLOCCULATING AGENT A POLYMER WITH A MOLECULAR WEIGHT OF FROM ONE MILLION TO TEN MILLION CONTAINING FROM 50 TO 80 MOLE PERCENT OF ACRYLAMIDE UNITS AND FROM 50 TO 20 MOLE PERCENT OF ANIONIC UNITS SELECTED FROM THE GROUP CONSISTING OF ACRYLIC ACID AND ACRYLATE UNITS.

2. A process according to claim 1, wherein said soluble phosphate salt is a sodium orthophosphate.

3. A process according to claim 1, wherein said soluble phosphate salt is added in an amount corresponding to from 100 to 600 parts by weight of P2O5 per million parts by weight of sugar in said liquor.

4. A process according to claim 3, wherein said soluble phosphate salt is added in an amount corresponding to from 200 to 400 parts by weight P2O5 per million parts by weight of sugar in said liquor.

5. A process according to claim 1, wherein said flocculating agent has a molecular weight of from four million to eight million.

6. A process according to claim 1, wherein from 1 to 20 parts by weight of said flocculating agent are used per million parts by weight of sugar in said liquor.

7. A process according to claim 1, wherein said mixture is retained in said flocculator vessel for a period of from 30 seconds to 3 minutes.

8. A process according to claim 1 wherein said flocculating agent is an acrylamide/acrylate copolymer having a molecular weight of about six million.

9. A process according to claim 8 wherein said flocculating agent has 40% anionic units.

10. A process according to claim 1 wherein said soluble phosphate salt is a sodium orthophosphate and is added in an amount corresponding to from 200-400 parts by weight of P2O5 per million parts by weight of sugar in said liquor, wherein said flocculating agent has a molecular weight of from four million to eight million and is employed in an amount from 1-20 parts by weight per million parts by weight of sugar in said liquor, and wherein said mixture is retained in said flocculator vessel for a period of from 30 seconds to 3 minutes.

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