CA1196916A - Removal of objectionable flavor and odor characteristics in finished sugar products produced from molasses - Google Patents

Abstract

REMOVAL OF OBJECTIONABLE FLAVOR AND ODOR
CHARACTERISTICS IN FINISHED SUGAR
PRODUCTS PRODUCED FROM MOLASSES

ABSTRACT OF THE DISCLOSURE

A method is disclosed whereby the sugar portion of ion excluded molasses is treated with a halogen or a nascent halogen agent in order to remove the objectionable flavor and odor characteristics normally associated with raw cane juice. The method generally comprises treating the sugar portion of ion excluded molasses according to the steps of:
a) subjecting the sugar portion of ion excluded molasses to gross decolorization;
b) purifying the solution treated according to step a) to remove all remaining impurities; and c) concentrating or evaporating the purified sugar portion so that the percent of dry solids in solution is substantially increased to obtain a high quality sugar product which conforms to or exceeds existing standards for such sugar products, the method being further characterized by subjecting the sugar portion prior to concentrating or evaporating to the steps comprising:
(i) treating the decolorized sugar portion obtained in step a) with a halogen or a nascent halogen agent so that the sugar portion is acidified to a point lower than its naturally occurring pH;
(ii) removing excess free halogen from the sugar portion treated according to step (i) to render the sugar portion free from objectionable flavor and odor characteristics.

Description

REMOVAL OF OBJECTIONABLE FLAVOR AND ODOR
CHARACTERISTICS IN FINISHED SUGA~
P~ODUCT~ PRODUCED FROM MOLASSES
. ...
BACRGROUND OF THE INVENTION

Histori~ally, khe sugar cane plan~ ha~ been cultivated for it~ ~weetness. This sweetness is a result of the rela~ively high concentration of sucro~e in the plantO Throughout history, man has worked to extrac~ and then purify the sucrose contained in raw cane juice by utilizing crystallization techniques which result in the production of raw sugar, molas~es~
or mixtures thereof.
~ eretofore~ ~radit;onal processing techniques have attempted to maximize the quantities of raw sugar when treating raw cane juice. The carbohydrate~
con~ained in the mo~asses have a lower economlc value when compared to the sugar contained in the raw sugar produced from cane juiceO The lower economic value of ~he carbohyarates contained in molasses is a result of the economic l~mitat~ons on extracting these ¢arbohy drates therefrom9 Current uses of the molasses include~ but are not limited to animal feeds, feedstock~ for certain chemical proce~se~ or ~he like~ Therefore~ it is prevalent in ~he indus~ry ~o maximize ~he production of raw sugar while minimizing the production of molasse~ to ~ake advantage of the higher economic value associated therewith~
Recently~ however~ certain processes have been dis~losed which enable the sugar~ present ln the 3D mola~se~ to be ~eparated Çrom the non sugar~ congained thereln in an econom~cal manner~ Such proces~e~ have been disclosed, for example9 in Unlted States Patent 3 ~ g75 ~ 205 and ~ni~ed States Patent 3 ~ 8 84 ~ 714 o ~hese , 1 ~ ~ 6.9~ ~

processes are generally referred to ln the lndustry as molas~e~ desugarization processesO In general term~, the molasses desugar~ tion process includes ` pretreating the mol~sses to lower the organic and : 5 inorganic non-sugars contained in the molasses, and separ~ting the sugar and non-sugar portions of the molasses by passing the molasses over sui~able ion exchange reslns according to ion exclusion techniques.
In the course of producing a finished sugar product from the sugar portion of the ion excluded molasses, it i~ essential that objectionable flavor and odor ch~racteristics are removed to ensure that the finished sugar product thus produced will meet or e~ceed ex;sting standards for such products~ It may be possible to achieve certain quantikies of ~uitabl~
fini~hed ~ugar product by passing the sugar portion of ion excluded molasses over conventional ion exchange materials~ such as~ for example, a~imal bone char~
commercia~ carbons~ carbonaceous adsorben~s or the likeO ~owever, these processes are economically disadvanta~eous due to the reduced volumes of acceptable finished sugar product obtained~
~ he nature of the sugar cane plant is such that the objectionable flavor and odor characteristics are inherent in the plant and are ~uch that the conventional methods described above are not adequa~e to completely remove the~e characteristics from a sugar product produced from ion excluded mola~sesO
Thus, whlle these inherent flavor and odor charac~eristics ~an be ~ubstantially removed through ~he u~e of the above-described conventional me~hods, the objectionable 1avor and odor characterist.~c~
remain in tr~ce amoun~ or greater even when ~uch conventional methods are utillzed~

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It has now been discovered tha~ the treatment of the sugar portion produced from the ion exclu~ion of molasses by a halogen or a cent halogen agent will completely r~mov~ even trace amounts of s objectional flavor and odor characteristics associated with the production of a finished ~ugar produ~t. The method according to the pres~nt invention i~ both economically feasible from a manufacturing viewpoint and produces a finished sugar product whlch conforms to or exceeds existing standards for such products.
~ eretofore, halogen or na~cent halogen agents have been used only as an oxidizing agent for the decoloration of ~ugar solutions, as for example, ~.S.
Patent Nos, 637~004î 1,591j879, 1,989D156 and 1~826,655. The chlorine disclosed in the ab~ve lis~ed - patents ~s generally utilized for the de olorization of raw sugar solu~ions such that crystalline sugar produced therefrom will be ~ubstantially color free.
Additiona~ly the chlorine may be utilized as a decolorizing agent according to the above patents when treating raw cane juice and producing raw sugar ~herefromO
Therefore~ it is a primary object of the present ~nvention to provide a high ~uality finlshed sugar produc~ which is completely $ree of the ob~ectionable flavor and odor ~haracteristics normally associated with cane juice which ~onforms to or exceed~ all existing standards for fin~shed sugar product~l It ~5 a further object o this invention to provide an economical method ~or r~moving th~
objectionable flavor and odor characteristics in a f~nished ~ugar produet produced from ~he desugar~zation of molasse~.

These and other objects of the present invention will be more appearent from the discussion whoch follows/.
SUMMARY OF THE INVENTION
The present invention further realtes to a process for producing a high-quality finished sugar product by treating the sugar portion of ion excluded molasses by a halogen or anascent halogen agent. The present invention provides for the addition of a halogen or a nascent such that the objectionable flavor processing steps such that the objhectionable flavor and odor characteristics normally asociated with raw cane juice are eliminatedl. These objectional flavor and odor compounds which are present in trace quantities in the finished sugar product may be removed completely by utilizing thge present invention. Thus, the key feature of the present invention is the addition or treatment of sugar-containing solutions in the form of sucrose, glucose, fructose, or mixtures thereof by a halogen or a nascent halogen agent. The finished sugar product which results is one that will conform to ror exceed all existing standards fro a high quality finished sugar prodivt.
Molasses desugarization enables sugar producers to separate the valuable carbohydrates from the organic and inorganic non-sugar portions. The sugar portion which contain these valuable carbohydrates can be fruther treated to produce a finished sugar product. It is the sugar portion of the ion excluded molasses which is preferably treated accirdubg ti tge present invention.

Methjods which may be utilized according to the present invention for mollasses desugarization generallu comprise the steps of:
a) producing raq sugar, molasses or mixtures thereof from raq cane juice;
b) separating the molasses from teh mixture of step a);
c) pretreating the separated molasses to substantially reduce the organic and inorganic non-sugar contents; and d) ion excluding the pretreated molasses which yields a sugar portion ans a non-sugar portion.
During the process of molasses desugarization to obtain a sugar and a non- sugar protion, it is necessary to introduce water prior to and durring the process steps of ion exclusion so that the sugra and nonsugar portions will be adequately separated. The sugar portion separated during ion exclusion will, thus, be aqu7eous in nature.
Thje present invention generally provices:
a) subjecting th sugar portion of ion excluded molasses to gross decolorization;
b) purifing the solution treated according tp step a) yp remove all remaining impurities; and c) concentratingf or evaporatijg the purified sugar portion so that the percent of dry solids in solution is substantilaly increased to obtain a high quality sugar product which conforms to or exceeds existing standards for such sugar products, the method being further characterized by subjecting the sugar portion prior to cincrntrating or evaporatijng to the steps comprising:
(i) treating the sugar portion with a halogen or nascent haloghe agent so that the sugar portion is acidified to a point lower that its naturally occuring pH;
(ii) remocing excess free halogen from the sugar portion treated accordint to step (i) to rendre the sugar portion free from objectionable flavor and odor charactreristics.
More specifivally, the preferred swquence of processing steps according to the present invention when treating the sugar portion of ion excluded molasses generally comprise:
a) subjecting the sugar portion of ion excluded molasses to gross decolorization;
b) treating the deolorized sugar portion qith a halogen or nascent halogen gent;
c) removing excess free halogen from teh halogen or nascent hlaogen treated sugar protion;
d) purifying the sugar portion treated acording to step c); and e) concentrating or evaporating the purifeic sugar portion to obtaon a high quality sugar product free from objectionable flavor and odor compounds which conforms to or ecxedds existing standards for a high quality finished sugar product.
While the process steps indicate the preferred sequence of the present invention, it should be understood thar the treatment of the sugar portion of ion excluded molasses with a halogen or a naxecent halpgen agemt cam occur at any time prior to concentration or evaporation. However, from an economical aspect, the halogen treatment preferably should occur at some point after teh molasses has been ioh excluded and sepearaed into th sugar and nonsugar portions so that the halogen or the nascent halogen agent is not unnecessarily exhausted in teh treatment of soil, dirt, foreign matter or excess impurities, includlng organic and inorganic nonsugars conta~ned in the molassesr DE:TAILED DESCRIPT:LON OF THE INVENTION
. .
Gross Decolorization ~he purpoæe of subjecting the sugar portlon of ion excluded molasses to gross decolori2ation i~ to subs~antially reduce ~he organic non-sugars con~ained ~her~in. ~ubjecting the sugar portion to such gross decolorization e~onomizes the addition of the halogen or the nascent halogen agent such that the agent will not be unnecesarily exhausted in treating excess impuri~ies including the organic and inorganic non-sugars.
The sugar portivn of the ion excluded molasses is subjected to gross decolorization by passing the sugar portion over an ion exchange resin which has the property of removing fxom the sugar portion the organic non sugar~ contained therein.
Various sui~able ion exchange resins exi~ in the industry, such as, for example, Rohm & Haas IRA 900.
Additionally~ other ac~eptable methods of gross decoloration exist ~uch as, subjecting the sugar portion to such material~ as animal bone char~
commercial carbons in ei~her powdered or granu~ar form, or carbonaceous adsorbent resin~.
The ~ugar portion of ion excluded molasses when subjected to the process of gross decolorlzation reduce3 the organic non-~ugars present thereln a~
color pigments and produces a substantially ~olorless : 30 solut~on~

~reatin~ with_a ~alo~en or a Nascent ~alo~en A~ent Treating the sugar portion of lon excluded molasses wi~h a halogen or a nascent halogen agent i~
an essential part of this i~ventlon. The purpose of treating the sugar portion according to the present lnvention i~ ~o completely eliminate objectionable flavor and odor charac~ersi~ti~ normally associated with raw cane ~uice. The treatment with a halogen or nascent halogen agent can~ theoretically, be accomplished at any time prior ~o evaporation or concentrationO However, as noted above, the presence of soil~ dirt, foreign matter, or excess impurities including organic and inorganic non-sugars in the molasses would unnecessarily exhaust the halogen or the nascent halogen agent, thereby increasing eostO
Therefore, the preferred embodiment of this invention i~ ~o treat ~he sugar portion o ~on excluded molasses with a halogen or a nascent halogen agent after the molas~es has been ion excluded~ and preferably af~er ~o the sugar portion has been subjected to gross decoloriza~îon~ but beore evaporation or concentration.
~ halogen agent as used according to the present inventlon can be in the form of a free halogen ~n the diatomiG molecular gaseous state, such as~ for example~ the diatomic molecules of 5hlorlne, bromine, lodine or fluorine, and preferably chlorine. ~hese diatomic ~olecular halogens in the ~aseous state exhibit ~imilar disassoci~tion properties when introduc2d lnto an aqueous ~olutionO A nascent halogen agen~ as used according to ~he presen~
inven~ion can be any compound thak will exhibat disassociation properti~ si~ilar to the dia~omic molecular halogens mentioned a~ve~ when ~uch nascent halogen ag~nt i5 introduced into an aqueou~

.

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6~iL6 g solution. Example~ of na~cen~ halogen agent~ which may be utilized according to the present lnvention are sodlum hypochlorite, calcium hypochlori~e or the like.

The halogen or nascent halogen agent utllized by the presen~ invention can b~, for example, chlorine gas, sodium hypochlorite, or the like. Preferably, chlorine gas i~ utilized and can be contacted with the ion exc~uded molasses susar por~ion in so~u~ion by any conventional industrial means ~uch as, gas injection, gas diffusion or the like. ~he sugar portion preferably should be ag;~ated or subjected to mezhanical mixing during the in~roduction of the gaseous chlorineD The solution will necessarily be acidifled upon the addition of the chlorine gas such 15 that th~ p~ of the solution is reduced to a value of not greater than 2.5, preferably 2.0~

It has ~hus been found ~ha~ when the sugar portion of ion excluded mola~ses is treated with a halogen or a nascent halogen agen~ such as r for example~ chlorine gas, according to the present invention, the trace quant~ties of objectionabl~

flavor and odor compounds normally associated with raw can juice are completely remvved from the finished sugar product therehy conforming to or exceeding existing standards for finished sugar pro~uct~, The resulting product is virtually odor free and exhibits a sweet taste with no objectionable flavor3 The p~ of the solut~on can be subsequently raised by any conventional method including the addltion of an alkaline agentD ~owever, ~t has been found that the solution p~ is ~atisactorily ral~ed during ~ub~e~uent purif~ation according to conventional lon exchange techniques. Rai~ng the ~%

of the solution in thi~ manner obYiates ~he use o an a~ditional chemica~ agent ~n the ~rea~ment o~ the 6.~

solution, and thu~, is the preferred method accordlng to the presen~ invention.

REMOVING EX OESS FREE ~ALOGEN

Due to the chemical incompatibil~ty of 5 certaln ion exchange resins wi th free halvgens, more specifically chlo~ine, i~ is necessary to remove ~he excess free halogen prior to passing the h~logen trea~ed solu~ion over ~uch ion exchange resin3 for ~he purpose of further purificat~on. The removal of free - 10 chlorine can be accomplished according to conventional technology by contacting the chlorine treated ~olution with activated carbons. The p~o~ess of removing excess free halogen by passing the halog2n treated solution over activated ~arbon has the additional advantage of removing a portion of the remaining organlc nonsugars such that the solution is further decolorlzed~

PURIFICATIO~

Purification is needed to effectively remov~
all re~aining impurities 50 as ~o produce a :Einished sugar produc~ that meets ox exceeds all eXiS~iR9 standards for pure sugar~ These standards specify that the sugar should be practically f~ee o~ color~
inorganic ash~ organic non-sugars~ undes~rAble odor~
and flavors, and visual particu~ate matter or ~edlment~
The followin~ procedure is offered ~l a guideline as ~o ~he ex~en~ o the treatment nece~ary to purtfy the ~ugar ~olut~on. Whil* this i~ by no means the only wa~ to ach~eve purificationj it 1~

6~ ~ ~

belleved that others will only be modifications of thi~ scheme. ~his scheme consists ofO
(1) Additional gro~s decolorization by use of decolorizing lon exchange resins;
~2) Filtration of the sugar solution to remove any visual particulate or sediment;
~3) Treatment of the ~ugar solution with animal bonP char, commercial carbons t~ranular or powdered) or carbonaceous adsorbent resins;
(4) Passing the solution over ca~ion/anion exchangers.

The ~reatment with a halogen or a nascent halogen agent as discussed above necessarily purifies the sugar ~olution with respe~t to the objectionable flavor and odor compounds according to thP present invention.

EVAPO~TION OR CONCENTRA'TION

The evaporatiQn or concentration step i5 carried out so as 'co in~rease 'chs dry solids level of the pure sugar to any desired degree and in preferably at least 70% in the inished product. Evaporatiorl can be accomplished by conventionally known techni~ues.
~here are several methods availa}:)le for cQmmerf~ial large ~cale evaporatlon, all of whi~h should be acceptable according to the present invention~
inc~uding~ bu~ no~ lirni~ed ~o~ liquid concentration and ~pray drying 9 EXAMPLE 1 (Comparative) A predetermined volume of the sugar portion obtained from ion excluded molaxxes produced according to conventional molasses desugarization methods was decolorized using a specific decolorizing resin. The molasses was passed directly over a commrecoa;
granular carbon adsorpttion chamber, ion exchanged and evaporated to yield a finished product typical of that obtained from utilizing conventional processes. The finished sugar product exhibited noticeable objetional flavor and odor characteristics.

An equal volume of the sugar portion obtained from ion excluded molasses to that examined in Example 1 above, was similarly decolorized using a specific decolorizing resin. However, in this example, the equal volume of the sugar portion until the pH of the chlorination with chlorint gas by bubnbling the gas directly throuhgh the sugar portion until the pH of the molasses was lowered to 2Ø Tje chlorinated molasses was subsequently passed directly over a commercial granual carbon adsorption chamber, ion exchanged and evaporated to yield a finished product in accordance with the present invention. The finished sugar product exhibited a neutral pH, or about 7Ø
Organoleptic evaluations of the finished sugar product prepared in accordance with this example dixclosed a complete absence of objectional flabor and odor characteristics normally associated with araw cane juice.
The invention habving been thus particularly and distinctly described , it will be appreciated thta ~ame may ~omprise~ consl~t or con~i~t essentially of ~he hereinabove recitea ~eps and ma~erials.
Furthermore~ ~hile the invention ha~ been herein aescribed in ~.,at ls presently conceived to be the : 5 most practical and preerred embodiment thereof, it will be apparent to those of ordlnary ~kill in the art ~hat modifica~ions may be made ~hereof within the scope of the invention, which ~cope is to be accorded ~he broadest interpreta~ion of the appended claim~ so 1~ aR to encompas~ all equivalent methods.

Claims (15)

WHAT IS CLAIMED IS:

1. A method for removing undesirable flavor and odor characteristi? in a finished sugar product produced from the ion exclusion of molasses which yields sugar and non sugar portions and wherein the sugar portion is treated according to the steps comprising:
a) subjecting the sugar portion of ion excluded molasses to gross decolorization;
b) purifying the solution treated according to step a) to remove all remaining impurities; and c) concentrating or evaporating the purified sugar portion so that the percent of dry solids in solution is substantially increased to obtain a high quality sugar product which conforms to or exceeds existing standards for such sugar products, the method being further characterized by subjecting the sugar portion prior to concentrating or evaporating to the steps comprising:
(i) treating the sugar portion with a halogen or a nascent halogen agent so that the sugar portion is acidified to a point lower than its naturally occurring pH;
(ii) removing excess free halogen from the sugar portion treated according to step (i) to render the sugar portion free from objectionable flavor and odor characteristics.

2. A method according to claim 1 wherein steps (i) and (ii) are practiced after subjecting the sugar portion to gross decolorization and prior to purifying.

3. A method according to claim 1 wherein the step (i) is carried out with chlorine gas.

4. A method according to claim 1 wherein the step (i) is carried out with a nascent halogen agent which is odium hypochlorite.

5. A method according to claim 1 wherein the solution treated according to step (i) is acidified so that the pH of said solution is between about 1.5 and 2.5.

6. A method according to claim 1 wherein the solution treated according to step (i) is acidified so that the pH of said solution is not greater than 2.5.

7. A method according to claim 1 wherein the solution treated according to step (i) is acidified so that the pH of said solution is 2Ø

8. A method according to claim 1 wherein step (ii) is carried out by passing the sugar portion over activated carbon.

9. A method according to claim 1 wherein gross decolorization according to step a) is accomplished by passing the sugar portion of ion excluded molasses over decolorizing resins.

10. A method according to claim 1 wherein step b) is practiced by subjecting the solution to filtration.

11. A method according to claim 1 wherein step b) is practiced by passing the solution through cation and anion exchange resins.

12. A method according to claim 1 wherein step c) is practiced by spray drying.

13. A method according to claim 1 wherein the percent of dry solids in solution evaporated or concentrated according to step c) is about 70%.

14. A method according to claim 3 wherein the chlorine gas is contacted with the sugar portion by directly injecting the chlorine in a gaseous state wherein.

15. A method according to claim 14 wherein the sugar portion is continuously agitated during the injection of gaseous chlorine.