April 29, 1952 I F. H.

BUCK EI'AL _ 2,594,863

CRYSTALLIZATION 0F SORBITOL
Filed Dec. 24. 1948 2 SHEETS—SHEET 2

_ Y FRANK. H. BUCK , -,
_} HQ 2 MICHAEL ‘M. LUSKIN,
- .pEaq . MARSHALL T. SANDERS
jrul INVENTORS
 Patented Apr. 29, 1952‘ 2,594,863

UNITED STATES" PATENT OFFICE

2,594,863 _

CRYSTALLIZATION 0F SORBITOL
Frank H. Buck, Brandywine Hundred, Michael M.
.Luskin, New Castle Hundred, and Marshall T.
Sanders, Brandywine Hundred,'Del., assignors
to Atlas Powder Company, Wilmington, Del., a
corporation of Delaware
Application December 24, 1948, Serial No. 67,202
5 Claims. (Cl. 260-637)
1 2 .
The present invention relates to the production one against another while propelling them
of sorbitol. through the zone. I
An object of the invention is the provision of a The process of the invention lends itself ad
method for the production of sorbitol in solid mirably to continuous operation in which granu
form. lar sorbitol is recycled through an elongated heat
Another object of the invention is the pro exchanging and mixing zone while molten sorbi
vision of a method for making crystalline sorbitol tol is added at the beginning of said zone and
in granular form. granular sorbitol is removed continuously or in
A further object of the invention is the pro increments from a point in the cycle outside of
vision of an improved method for the produc 10 the cooling and mixing zone. The invention will
tion of a dry crystalline sorbitol. be further described in terms of one device for
still another object of the invention is the pro conducting such a continuous process and in
vision of an advantageous method for producing connection with the drawings in which:
dry crystalline sorbitol in granular form directly I Figure 1 is a diagrammatic longitudinal view,
from a sorbitol melt. , 15 partly in section, of an apparatus for perform
Other objects will be apparent from the fol ing the invention;
lowing description, Figure 2 is a sectional end view‘of the appa
Sorbitol is customarily produced in aqueous so ratus of Figure 1 taken on line 2-2 of Figure 1,
lution by the hydrogenation of aqueous solutions and
of glucose, and it is largely marketed in solution 20 Figure 3 is an end view taken from the left
form. For many purposes, however, it is de end of Figure 1.
sirable that sorbitol be in dry granular form. Referring to the ?gures in detail, ll designates
Processes have been developed for growing generally an elongated jacketed mixer including
crystals of sorbitol in solution and either sepa outside shell I5 and inside shell l9,' and?tted
rating such crystals from their mother liquor 25 with a removable cover H3. The bottom of in
for drying, or dryingthe magma of crystals and side shell I!) is divided into ‘two arcuateportions
mother liquor , in such manner that the re 23 and 21. A series of ports,_one of which is
mainder of the sorbitol crystallizes as the sol shown as, 28, provide ingress for heat exchange
vent evaporates. However, such procedures are fluid to the jacket formed by shells l5 andvl9.
expensive and time consuming, involving di?i 30 The said ?uid leaves the jacket through a similar
cultly controlled procedures or the use of ex series of ports, one of which is shown as 29, on the
pensive equipment. ' opposite side of the mixer. A bottom outlet in
Direct production of granular sorbitol from ‘ the jacket for draining may be provided at 26.
moltenisorbitol such as may be obtained by Shafts 3| and 35 extend longitudinally in side
evaporating an aqueous solution thereof to vir 35 by-side relationship through mixer ll. Shaft 3|
tual dryness has not heretofore been found prac- ' is journaled in bearings 38 and 43 and is pro
tical because of the hygroscopic nature of sorbi vided with paddles along its length. Thev paddles
tol, and because of its tendency on cooling from generally designated by 4'! are adjustable in
'a'melt to set up as a body into a hard glassy con pitch and are so adjusted as to provide both a
mixing and propulsive action (from left to right
dition. '
40 in the apparatus shown in Figure 1). , Shaft 3|
_ In accordance with the present invention
granular'sorbitol may be produced from molten is provided on one end with gear wheel 5|. Shaft
sorbitol if the molten material is mixed with pre 35 (see Figures 2 and 3) is provided with paddles
formed grains of crystalline sorbitol, and the 55, and bearings, one of which is shown as 39, and
a gear (not shown) similar to those provided for
mixture is further mixed with preformed dry 45 shaft 3|. The gears mesh so that turning of
grains of crystalline sorbitol while heat of crys shaft 3| makes shaft it turn in the opposite di
tallization is abstracted from the mixture. rection. Shaft 3| may be driven by any suitable
Desirably the performance of these steps may means (not shown). v
be carried out by feeding preformed granular Conveyer 85 elevates granular sorbitol from the
crystalline sorbitol and molten sorbitol into an 50
discharge end of mixer ll, whence it may be
elongated heat exchanging zone containing pre either recycled to the mixer by means of chute 65
formed grains of crystalline, granular sorbitol or removed from the system to storage by means
and agitating and mixing means, such as paddles, of chute 13 depending upon the setting of the
‘ which forcibly mix the granules, rubbing them 55 movable vane 89. Granular sorbitol is dis
 2,594,863
3 {A
charged from mixer H through ports 16and 11 invention. For example, some crystallization
from which it falls into duct BI and is delivered to may occur in the ?rst, and undoubtedly occurs in
the base of the elevating conveyer 85. the second zone since the solids in the mixer are
Spray head 89, through which molten sorbitol at all times below the melting point of sorbitol.
is introduced into the apparatus is mounted However, by‘ the arrangement described, any
above the center line of the elongated mixer, thick ?lms of viscous, super-cooled sorbitol melt
just down stream from the point at which pre through which crystallization would proceed very
formed granular crystalline sorbitol enters slowly are removed from the zone in which more
through duct 65. Molten sorbitol is conducted‘ liquid phase is added and are rubbed and tum
to the spray head 89 through pipe 553 from a 10 bled against uncoated granules whereby the
source not shown. ?lms are thinned down and thoroughly subjected
In operation the apparatus is partially ?lled to the seeding action of the crystalline material
with crystalline sorbitol in granular form. Then. in the preformed granules. The rate of addition
with shafts 3i and 35 being driven slowly so that of molten sorbitol relative to the rate and
paddles 41 and 55 thoroughly mix the contents - amount of granular material being recycled is
of mixer II and slowly propel them toward exit kept sufficiently low that the formation of a
ports 76 and T1, preformed granular sorbitol is matrix about the granules is avoided. Crystal
fed to mixer H through duct 65, and molten lization is thus hastened and by the time a given
sorbitol is sprayed onto the agitated granular portion of the circulating material has completed
sorbitol. Meanwhile, the apparatus is main 20 its cycle the surface layer has crystallized to
tained at a proper crystallization temperature by such an extent that it can serve as seed to induce
means of heat exchange ?uid ?owing through crystallization in a fresh ?lm of molten sorbitol.
the jacket formed by shells l5 and I9. The following example illustrates a speci?c
The granular sorbitol produced in the process embodiment of the process of the invention.
together with that originally present passes out 25
the exit ports 16 and ‘H into duct 8i and from Example
thence to conveyor 85 by means of which it is A mixer of the type described and having
fed back to the apparatus through duct 55 or about 100 paddles regularly spaced through about
directed to product storage through chute 13 131/2 feet of mixing length was operated with a
depending upon the position selected for vane 30 base load of about 3,000 lbs. of granular sorbitol.
69. Vane 69 is turned to recycle the granular Molten sorbitol which had been evaporated so
sorbitol until the amount of material in the that it had a water content of about 0.5% was
mixer builds up to a predetermined extent. Then fed into the apparatus at a temperature of 220° F.
vane 69 is turned to direct the granular sorbitol and at a rate of 360 pounds per hour. The tem
to product storage until the excess is taken off, 35 perature of the heat exchange fluid in the jacket
after which it is returned to recycle position. Of was regulated to keep the mass of material in the
course, means may be provided so that granular mixer at about 180° F. The shafts were turned
sorbitol may be drawn o? continuously at a rate at a rate of 8 R. P. M. and the paddles were
equal to that at which molten sorbitol enters the adjusted so that 9,660 pounds per hour of mate
mixer, but the arrangement shown has been rial left the apparatus. All of the material leav
found satisfactory. ing the apparatus was either recycled or passed
The molten sorbitol admitted to the apparatus, to storage in a repeated cycle of 40 minutes dur
being viscous, heavily coats the top layer of ing which all material was recirculated and 1.6
granules of crystalline sorbitol which it ?rst minutes during which all material was sent to
contacts. vThen the mixing and propulsion 45 product storage. The bulk of the granular sor
caused by the paddles makes the coated granules bitol emerging from the apparatus (and hence
rub against fresh uncoated granules, and the the granular material being recycled) had a
molten sorbitol is spread into a very thin film, in grain size ranging from about 1/: inch to about
contact with crystalline sorbitol on both sides % inch in diameter.
of the ?lm and subjected to mechanical working. 50 As has been mentioned. above, the process of the
These conditions favor rapid crystallization of invention is particularly valuable because it pro
the molten ?lm. Simultaneously a suiiicient' vides a means of forming a granular product
number of projecting irregularities and parasite from molten sorbitol. It is not meant to imply,
crystals are broken from the granules to form however, that the sorbitol used must be absolute
nuclei for new grains. Unexpectedly, a dispro 55 ly dry, for the process may be satisfactorily ap
portionate share of the sorbitol melt seems to’ plied to sorbitol having water contents up to
adhere to such smaller irregularly shaped grains about 2%. As the water content exceeds this
rather than to larger, smooth granules or pellets, value, however, the process becomes less prac
and there is little tendency for the average parti tical, for the product becomes progressively
cle size to increase even after long continued 60 stickier and more di?icult to handle.
operation. The temperature at which the body of material
The sequence of steps involved in the process being mixed is maintained can be varied. Too
of the invention may be summarized as follows. low a temperature, below about 120° F., retards
In aw ?rst zone of the apparatus, immediately the rate of crystallization in the ?lm of molten
under spray head 88, preliminary mixing of 65 sorbitol, probably because of the resultant high
molten and granular sorbitol andthe coating of viscosity thereof. It is necessary, however, that
some of the granular sorbitol with molten sor the temperature of the grains be sufficiently low
bitol takes place. In the central portion of the to cool the molten sorbitol to a temperature below
elongated. mixer, mixing and‘ rubbing of coated its melting point. The preferred range is between
material with uncoated granular sorbitol occurs. about 160° F. and about 195° F. '
In the third zone, toward the" exit ports 16 and . ‘ The desirability of spreading the molten sor
11, occurs ?nal crystallization and formation of bitol in a thin ?lm over and between granules
the new solid sorbitol. These zones are not, it of crystalline sorbitol in the mixer and of avoid
will be appreciated, clearly‘ de?ned, but they indie , ing the formation of a matrix have been pointed
cate generally the course of the process of the 75 out, and in order to supply a su?icient surface '
 2,594,863
5 6
area of granules it is desirable that the ratio of bitol to said elongated zone being insu?icient to
recycled solid phase to feed of molten sorbitol be provide a matrix about said granules after mix
greater than about 10 to 1 and preferably be ing; discharging granular crystalline sorbitol
maintained at above about 15 to 1. At lower from theafter end of the elongated zone after
ratios inordinately long times for complete UK the added molten sorbitol has substantially
crystallization of the melt may be encountered. crystallized; and maintaining the temperature
Higher ratios may be utilized although there in the said elongated zone above about 120° F.
seems to be no practical advantage in recircu and below the melting point of sorbitol.
lating more than about 30 pounds of solid for each 2. A process as described in claim 1 in which
pound of feed introduced. 10 the weight of granular crystalline sorbitol enter
The length of time between successive coatings ing the said elongated zone per unit time is at
of a granule with molten sorbitol is controlled by. least ten times the weight of said molten sorbitol
the ratio of weight recycled per unit time to the added per unit time.
weight of granular sorbitol in the system. De 3. A process as described in claim 1 in which
sirably, a residence time in the mixer of at least the temperature of the material in the said elon
10 minutes is allowed which is achieved by re gated zone is maintained between about 160" F.
cycling a maximum of 6 pounds per hour for and about 195° F.
each pound of granular sorbitol in process. Pref 4. A process as described in claim 1 in which
erably a time of at least 15 minutes is allowed the residence time of the mixture of granular
which may be achieved by maintaining the ratio 20 crystalline sorbitol and molten sorbitol in the said
of pounds recycled per hour to pounds in process elongated zone is at least 10 minutes.
at a maximum value of 4. Longer residence 5. A process for preparing granular crystalline
times, achieved by decreasing this ratio, are in sorbitol which comprises continuously advancing
no wise detrimental to the process except as they a body of preformed granules of crystalline sor
limit the amount of product produced in a mixer bitol in a cycle which includes an elongated zone,
of given holding capacity by virtue of limitation the rate‘of advance being such that the residence
on the ratio of recycled material to feed of molten time in the said elongated zone is at least 10
sorbitol disclosed above. minutes; intimately mixing and rubbing the
In terms of the just discussed ratios the ex granules one against another in said elongated
ample cited above Was operated at a ratio of re zone; adding molten sorbitol containing not more
cycled granular sorbitol to feed of 26.7 and at than about 2 percent water at the beginning of
a ratio of recycled material per hour to material said elongated zone at a rate in terms of weight
in process of 3.2. per unit time not to exceed one tenth of the rate
The temperature of the molten sorbitol fed to at which the said body of granular sorbitol enters
the mixer must be above about 198° F. to avoid the elongated zone; withdrawing crystalline sor
risk of freezing and congealing in the lines and bitol from a point outside of said elongated zone;
is expediently maintained below about 230° F. and maintaining the material in the elongated
to avert risk of developing odor and color by zone at a temperature between about 160° F. and
thermal degradation. about 185° F.
What is claimed is: FRANK H. BUCK.
1. A process for preparing granular crystal MICHAEL M. LUSKIN.
line sorbitol which comprises advancing a body MARSHALL T. SANDERS.
of ~preformed granules of crystalline sorbitol
through an elongated zone in which the gran REFERENCES CITED
ules are forcibly mixed and rubbed one against The following references are of record in the
another; adding molten sorbitol containing not ?le of this patent:
more than about 2 percent water to the forepart
of said elongated zone; distributing said molten UNITED STATES PATENTS
sorbitol over said granules in said forepart and Number Name Date
in a subsequent part of said elongated zone by 2,091,900 Widmer __________ __ Aug. 31, 1937
said forcible mixing and rubbing action among ‘ 2,315,699 Goepp_____________ __ Apr. 6, 1943
the granules; the rate of addition of molten sor 2,347,288 Schlegel et al. ______ Apr. 25, 1944