Note: Descriptions are shown in the official language in which they were submitted.
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~
~6~
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.
5
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~
.
. ~
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
12
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.
EXAMPLE 2
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
13
~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.
