Note: Descriptions are shown in the official language in which they were submitted.
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WO 98/14558 PCT/US97/09796
PROCESS FOR MAKING A DETERGENT COMPOSITION BY NON-TOWER
PROCESS
10 FIELD OF THE INVENTION
The present invention generally relates to a non-tower process for
producing a particulate detergent composition. More particularly, the
invention is
directed to a continuous process during which detergent agglomerates are
produced by feeding a surfactant and coating materials into a series of
mixers.
I S The process produces a free flowing, detergent composition whose density
can
be adjusted for wide range of consumer needs, and which can be commercially
sold.
BACKGROUND OF THE INVENTION
Recently, there has been considerable interest within the detergent
20 industry for laundry detergents which are "compact" and therefore, have low
dosage volumes. To facilitate production of these so-called low dosage
detergents, many attempts have been made to produce high bulk density
detergents, for example with a density of 600 g// or higher. The low dosage
detergents are currently in high demand as they conserve resources and can be
25 sold in small packages which are more convenient for consumers. However,
the
extent to which modem detergent products need to be "compact" in nature
remains unsettled. In fact, many consumers, especially in developing
countries,
continue to prefer a higher dosage levels in their respective laundering
operations.
30 Generally, there are two primary types of processes by which detergent
granules or powders can be prepared. The first type of process involves spray-
drying an aqueous detergent slurry in a spray-drying tower to produce highly
porous detergent granules (e.g., tower process for low density detergent
compositions). In the second type of process, the various detergent components
35 are dry mixed after which they are agglomerated with a binder such as a
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_2_
nonionic or anionic surfactant, to produce high density detergent compositions
(e.g., agglomeration process for high density detergent compositions). In the
above two processes, the important factors which govern the density of the
resulting detergent granules are the shape, porosity and particle size
distribution
of said granules, the density of the various starting materials, the shape of
the
various starting materials, and their respective chemical composition.
There have been many attempts in the art for providing processes which
increase the density of detergent granules or powders. Particular attention
has
been given to densification of spray-dried granules by post tower treatment.
For
example, one attempt involves a batch process in which spray-dried or
granulated detergent powders containing sodium tripoiyphosphate and sodium
sulfate are densified and spheronized in a Marumerizer~. This apparatus
comprises a substantially horizontal, roughened, rotatable table positioned
within
and at the base of a substantially vertical, smooth walled cylinder. This
process,
however, is essentially a batch process and is therefore less suitable for the
large scale production of detergent powders. More recently, other attempts
have
been made to provide continuous processes for increasing the density of "post-
tower" or spray dried detergent granules. Typically, such processes require a
first apparatus which pulverizes or grinds the granules and a second apparatus
which increases the density of the pulverized granules by agglomeration. While
these processes achieve the desired increase in density by treating or
densifying
"post tower" or spray dried granules, they are limited in their ability to go
higher
in surfactant active level without subsequent coating step. In addition,
treating or
densifying by "post tower" is not favourable in terms of economics (high
capital
cost) and complexity of operation. Moreover, all of the aforementioned
processes are directed primarily for densifying or otherwise processing spray
dried granules. Currently, the relative amounts and types of materials
subjected
to spray drying processes in the production of detergent granules has been
limited. For example, it has been difficult to attain high levels of
surfactant in the
resulting detergent composition, a feature which facilitates production of
detergents in a more efficient manner. Thus, it would be desirable to have a
process by which detergent compositions can be produced without having the
limitations imposed by conventional spray drying techniques.
To that end, the art is also replete with disclosures of processes which
entail agglomerating detergent compositions. For example, attempts have been
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WO 98/14558 PCTlUS97/09796
made to agglomerate detergent builders by mixing zeolite and/or layered
silicates in a mixer to form free flowing agglomerates. While such attempts
suggest that their process can be used to produce detergent agglomerates, they
do not provide a mechanism by which starting detergent materials in the form
of
pastes, liquids and dry materials can be effectively agglomerated into crisp,
free
flowing detergent agglomerates.
Accordingly, there remains a need in the art to have an agglomeration
(non-tower) process for continuously producing a detergent composition having
high density delivered directly from starting detergent ingredients, and
preferably
the density can be achieved by adjusting the process condition. Also, there
remains a need for such a process which is more efficient, flexible and
economical to facilitate large-scale production of detergents (1) for
flexibility in
the ultimate density of the final composition, and {2) for flexibility in
terms of
incorporating several different kinds of detergent ingredients, especially
detergent ingredients in the form of liquid, into the process.
The following references are directed to densifying spray-dried granules:
Appel et al, U.S. Patent No. 5,133,924 (Lever); Bortolotti et al, U.S. Patent
No.
5,160,657 (Lever); Johnson et al, British patent No. 1,517,713 (Unilever); and
Curtis, European Patent Application 451,894.
The following references are directed 'to producing detergents by
agglomeration: Beujean et al, Laid-open No.W093/23,523 (Henkel), Lutz et al,
U.S. Patent No. 4,992,079 (FMC Corporation); Porasik et al, U.S. Patent No.
4,427,417 (Korex); Beerse et al, U.S. Patent No. 5,108,646 (Procter 8 Gamble);
Capeci et al, U.S. Patent No. 5,366,652 (Procter & Gamble); Holiingsworth et
al,
European Patent Application 351,937 (Unilever); Swatting et al, U.S. Patent
No.
5,205,958; Dhalewadikar et al, Laid Open No.W096/04359 (Unilever).
For example, the Laid-open No.W093/23,523 (Henkel) describes the
process comprising pre-agglomeration by a low speed mixer and further
agglomeration step by high speed mixer for obtaining high density detergent
composition with less than 25 wt% of the granules having a diameter over 2
mm. The U.S. Patent No. 4,427,417 (Korex) describes continuous process for
agglomeration which reduces caking and oversized agglomerates.
None of the existing art provides all of the advantages and benefits of the
present invention.
CA 02267424 2002-O1-28
SUMMARY OF THE INVENTION
The present invention meets the aforementioned needs in the art
by providing a process which produces a high density granular detergent
composition. The present invention also meets the aforementioned
needs in the art by providing a process which produces a granular
detergent composition for flexibility in the ultimate density of the final
composition from agglomeration (e.g., non-tower) process. The process
does not use the conventional spray drying towers currently which is
limited in producing high surfactant loading compositions. In addition, the
process of the present invention is more efficient, economical and flexible
with regard to the variety of detergent compositions which can be
produced in the process. Moreover, the process is more amenable to
environmental concerns in that it does not use spray drying towers which
typically emit particulates and volatile organic compounds into the
atmosphere.
As used herein, the term Gagglomerates" refers to particles formed
by agglomerating raw materials with binder such as surfactants and/or
inorganic solutions/organic solvents and polymer solutions. As used
herein, the term "granulating" refers to fluidizing agglomerates thoroughly
for producing free flowing, round shape granulated-agglomerates. As
used herein, the term "mean residence time" refers to following definition:
mean residence time (hr) = mass (kg)/flow throughput (kg/hr)
All percentages used herein are expressed as "percent-by-weight"
unless indicated otherwise. All ratios are weight ratios unless indicated
otherwise. As used herein, comprising" means that other steps and
other ingredients which do not affect the result can be added. This term
encompasses the terms "consisting of° and Nconsisting essentially ofn.
In accordance with one aspect of the invention, there is provided a
non-tower process for preparing a granular detergent composition having
a density of at least about 600g/1, comprising the steps of: (a) dispersing
i
CA 02267424 2002-08-15
-5-
a surfactant, and coating the surfactant with fine powder having a diameter
from 0.1 to 500 microns, in a first mixer wherein conditions of the first
mixer
include (i) from about 2 to about 50 seconds of mean residence time, (ii) from
about 4 to about 25 m/s of a tip speed, and (iii) from about 0.15 to about 7
kjlkg
of energy condition, wherein first agglomerates are formed; (b) spraying
finely
atomized liquid onto the first agglomerates in a second mixer wherein
conditions of the second mixer include (i) from about 0.2 to about 5 seconds
of
mean residence time, (ii) from about 10 to about 30 m/s of tip speed, and
(iii)
from about 0.15 to about 5 kj/kg of energy condition, wherein second
agglomerates are formed; (b') thoroughly mixing the second agglomerates in a
third mixer affixed with choppers which break up oversized agglomerates and
wherein conditions of the third mixer include (i) from about 0.5 to about 15
minutes of mean residence time and (ii) from about 0.15 to about 7 kj/kg of
energy condition, wherein third agglomerates are formed; and (c) granulating
the third agglomerates in one or more fluidizing apparatus in the presence of
droplets of an aqueous silicate solution wherein conditions of each of the
fluidizing apparatus include (i) from about 1 to about 10 minutes of mean
residence time, (ii) from about 100 to 300 mm of depth of unfluidized bed,
(iii)
not more than about 50 micron of droplet spray size of said aqueous silicate
solution, (iv) from about 175 to about 250 mm of spray height of said aqueous
silicate solution above a distributor plate of said fluidizing apparatus, (v)
from
about 0.2 to about 1.4 m/s of fluidizing velocity and (vi) from about
12° to about
100°C of bed temperature.
Also provided are the granular detergent compositions having a high
density of at least about 600g/1, produced by any one of the process
embodiments described herein.
Accordingly, it is an object of the invention to provide a process for
continuously producing a detergent composition which has flexibility with
respect to density of the final products by controlling energy input,
residence
time condition, and tip speed condition in the mixers. It is also an object of
the invention to provide a process which is more efficient,
CA 02267424 2002-O1-28
flexible and economical to facilitate large-scale production. These and
other objects, features and attendant advantages of the present invention
will become apparent to those skilled in the art from a reading of the
following detailed description of the preferred embodiment and the
appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flow diagram of a process in accordance with one
embodiment of the invention which includes the agglomeration process
by the first mixer, followed by the second mixer, then fluidizing apparatus,
to produce a granular detergent composition having a density of at least
600g/1.
FIG. 2 is a flow diagram of a process in accordance with one
embodiment of the invention which includes the agglomeration process
by the first mixer, followed by the second mixer, then the third mixer,
finally fluidizing apparatus, to produce a granular detergent composition
having a density of at feast 600g/1.
FIG. 3 is a flow diagram of a process which is capable to conduct
variety of agglomeration processes selected from the group consisting of
the first mixer, the second mixer, the third mixer, fluidizing apparatus, and
the combination thereof, to produce a granular detergent composition.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is directed to a process which
produces free flowing, granular detergent agglomerates having
a density of at least about 600g/1. The process produces
granular detergent agglomerates from an aqueous
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_7_
and/or non-aqueous surfactant which is then coated with fine powder having a
diameter from 0.1 to 500 microns, in order to obtain low density granules.
Process
Reference is now made to Fig.1 which presents a flow chart illustrating
an embodiment of the present invention, i.e., process comprising the first
step,
the second step (i) and the third step below; and Fig.2 which presents a flow
chart illustrating an embodiment of the present invention, i.e., process
comprising the first step, the second steps (i) and (ii), and the third step
below.
Another reference is now made to Fig.3 which presents a flow chart
illustrating
various embodiments which include the present invention.
First Step (Step(a)1
In the first step of the process, surfactant 11, i.e., one or more of aqueous
and/or non-aqueous surfactant(s), which is/are in the form of powder, paste
and/or liquid , and fine powder 12 having a diameter from 0.1 to 500 microns,
preferably from about 1 to about 100 microns are fed into a first mixer 13, so
as
to make agglomerates. (The definition of the surfactants and the fine powder
are
described in detail hereinafter.) Optionally, an internal recycle stream of
powder
30, having a biameter of about 0.1 to about 300 microns generated from
fluidizing apparatus 27, which are described hereinafter in the step 3, can be
fed
into the mixer in addition to the fine powder. The amount of such internal
recycle
stream of powder 30 can be 0 to about 60 wt% of final product 29.
In another embodiment of the invention, the surfactant 11 can be initially
fed into a mixer or pre-mixer (e.g. a conventional screw extruder or other
similar
mixer) prior to the above, after which the mixed detergent materials are fed
into
the first step mixer as described herein for agglomeration.
Generally speaking, preferably, the mean residence time of the first mixer
is in range from about 2 to about 50 seconds and tip speed of the first mixer
is in
range from about 4 m/s to about 25 mls, the energy per unit mass of the first
mixer (energy condition) is from about 0.15 kj/kg to about 7 kj/kg, more
preferably, the mean residence time of the first mixer is in range from about
5 to
about 30 seconds and tip speed of the first mixer is in range from about 6 m/s
to
about 18 mls, the energy per unit mass of the first mixer (energy condition)
is in
range from about 0.3 kj/kg to about 4 kj/kg, and most preferably, the mean
residence time of the first mixer is in range from about 5 to about 20 seconds
CA 02267424 2002-O1-28
~8-
and tip speed of the first mixer is in range from about 8 mls to about 18 mls,
the
energy per unit mass of the first mixer (energy condition) is in range from
about
0.3 kj/kg to about 4 kjlkg.
The examples of mixers for the first step can be any types of mixer known
to the skilled in the art, as long as the mixer can maintain the above
mentioned
condition for the first step. An Example can be L~dige CB Mixer manufactured
by the Lt~dige Company (Germany). As the result of the first step, the
resultant
product 16 (first agglomerates having fine powder on the surface of the
agglomerates) is then obtained.
t0 Second Step (Step (b] I Steo (bbl
As one preferred embodiment, there are two types of choice, i.e., second
step (t) only, or second step (t) followed by second step (ii).
Second Steo (t) jSteglbll: The resultant product 16, i.e., the first
agglomerates, is fed into a second mixer 17, and then finely atomized liquid
18 is
sprayed on the first agglomerates in the mixer 17. Optionally, excessive fine
powder formed in the first step is added to the second step. If the excessive
fine
powder is added to the second step (t), spraying the finely atomized liquid is
useful in order to bind the excessive fine powder onto the surface of
agglomerates. About 0-10% , more preferably about 2-5% of powder detergent
ingredients of the kind used in the first step andlor other detergent
ingredients
can be added to the mixer 17.
Generally speaking, preferably, the mean residence time of the second
mixer is in range from about 0.2 to about 5 seconds and tip speed of the mixer
of
the second mixer is in range from about 10 m/s to about 30 m/s, the energy per
unit mass of the second mixer (energy condition) of the second mixer is in
range
from about 0.15 kjlkg to about 5 kjlkg, more preferably, the mean residence
time
of the second mixer is in range from about 0.2 to about 5 seconds and tip
speed
of the second mixer is in range from about 10 mls to about 30 mJs, the energy
per unit mass of the second mixer (energy condition) is in range from about
0.15
kjlkg to about 5 kj/kg, the most preferably, the mean residence time of the
second mixer is in range from about 0.2 to about 5 seconds, tip speed of the
second mixer is in range from about 15 mls to about 26 mls, the energy per
unit
mass of the second mixer (energy condition) is from about 0.2 kjlkg to about 3
kjlkg.
CA 02267424 2002-O1-28
.9.
The examples of the second mixer 17 can be any types of mixer known to
the skilled in the art, as long as the mixer can maintain the above mentioned
condition for the second step (i). An Example can be FlexomicMModel
manufactured by the Schugi Company (Netherlands). As the result of the second
step, the resultant product 20, is then obtained. The resultant product 20
(second agglomerates) is then subjected to either the second step (ii) or the
third
step.
Second Step (ill tSte~ fb'~y The resultant product 20 (second
agglomerates) of the second step (i) is fed into a third mixer 21. Namely, the
resultant product from the second mixer is mixed and sheared thoroughly for
rounding and growth of the agglomerates in the third mixer 21. Optionally,
about
0-10% , more preferably about 2-5°~ of powder detergent ingredients of
the kind
used in the first step andlor the second step (i), and/or other detergent
ingredients can be added to the second step (ii). Preferably, choppers which
are
attachable for the third mixer can be used to break up undesirable oversized
agglomerates. Therefore, the process including the third mixer 21 with
choppers
is useful in order to obtain reduced amount of oversized agglomerates as final
products, and such process is one preferred embodiment of the present
invention.
Generally speaking, preferably, the mean residence time of the third mixer
is in range from about 0.5 to about 15 minutes and the energy per unit mass of
the third mixer (energy condition) is in range from about 0.15 to about 7
kjlkg,
more preferably, the mean residence time of the third mixer is from about 3 to
about 6 minutes and the energy per unit mass of the third mixer (energy
condition) is in range from about 0.15 to about 4kjlkg.
The examples. of the thins mixer 21 can be any types of mixer known to
the skilled in the art, as long as the mixer can maintain the above mentioned
condition for the second step (ii). An Example can be LtSdige KM Mixer
manufactured by the LBdige company (Germany). As the result of the second
step (ii), the resultant product 24, i.e., granules with round shape is then
obtained.
Third S~eo t Steo (c)1
In the third step of the process, the resultant product of the second step,
i.e., a resultant product 20 or a resultant product 24, is fed into a
fluidized
apparatus 27, such as fluidized bed, in order to enhance granulation for
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WO 98114558 PCT/US97109796
-10-
producing free flowing high density granules. The third step can proceed in
one
or more than one fluidized apparatus (e.g., combining different kinds of
fluidized
apparatus such as fluid bed dryer and fluid bed cooler ). tn the third step,
the
resultant product from the second step is fluidized thoroughly so that the
granules from the third step have a round shape. Optionally, about 0 to about
10% , more preferably about 2-5% of powder detergent materials of the kind
used in the first step and/or other detergent ingredients can be added to the
third
step. Also, optionally, about 0 to about 20%, more preferably about 2 to about
10% of liquid detergent materials of the kind used in the first step, the
second
step and/or other detergent ingredients can be added to the step, for
enhancing
granulation and coating on the surface of the granules.
Generally speaking, to achieve the density of at least about 600 g//,
preferably more than 650811, condition of a fluidized apparatus can be;
Mean residence time : from about 1 to about 10 minutes
i 5 Depth of unfluidized bed : from about 100 to about 300 mm
Droplet spray size : not more than about 50 micron
Spray height: from about 175 to about 250 mm
Fluidizing velocity : from about 0.2 to about 1.4 m/s
Bed temperature : from about 12 to about 100 °C,
more preferably;
Mean residence time : from about 2 to about 6 minutes
Depth of unfluidized bed : from about 100 to about 250 mm
Droplet spray size : less than about 50 micron
Spray height: from about 975 to about 200 mm
Fluidizing velocity : from about 0.3 to about 1.0 m/s
Bed temperature : from about 12 to about 80 °C.
If two different kinds of fluidized apparatus would be used, mean
residence time of the third step in total can be from about 2 to about 20
minutes,
more preferably, from about 2 to 12 minutes.
A coating agent to improve flowability andlor minimize over agglomeration
of the detergent composition can be added in one or more of the following
locations of the instant process: (1 ) the coating agent can be added directly
after
the fluid bed cooler or fluid. bed dryer; (2) the coating agent may be added
between the fluid bed dryer and the fluid bed cooler; and/or (3) the coating
agent
may be added directly to the third mixer 21 and the fluid bed dryer. The
coating
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WO 98!14558 PCT/US97/09796
_11_
agent is preferably selected from the group consisting of aluminosilicates,
silicates, carbonates and mixtures thereof. The coating agent not only
enhances
the free flowability of the resulting detergent composition which is desirable
by
consumers in that it permits easy scooping for detergent during use, but also
serves to control agglomeration by preventing or minimizing over
agglomeration.
As those skilled in the art are well aware, over agglomeration can lead to
very
undesirable flow properties and aesthetics of the final detergent product.
In the case that the process of the present invention is carried out by
using (1) CB mixer which has flexibility to inject at least two liquid
ingredients; (2)
Schugi Mixer which has flexibility to inject at least two liquid ingredients;
(3) KM
mixer which has flexibility to inject at least a liquid ingredient; (4)
Fluidized (Fluid)
Bed which has flexibility to inject at least two liquid ingredients, the
process can
incorporate seven different kinds of liquid ingredients in the process.
Therefore,
the proposed process is beneficial for persons skilled in the art in order to
incorporate into a granule making process starting detergent materials which
are
in liquid form and are rather expensive and sometimes more difficult in terms
of
handling and/or storage than solid materials.
The proposed invention is also useful in view of industrial requirement,
because the person skilled in the art can set a series of apparatuses (e.g.,
shown in the Fig. 3) in a plant, and by using divertors which are capable for
connecting/disconnecting between each apparatus, so that the skilled in the
art
can select variations of the process to meet desired property (e.g., particle
size,
density, formula design) of the final product. Such variations include not
only
the process of the present inventions, i.e., shown as in the Fig. 3, (i) First
Mixer
13 - (fine 16) - Second Mixer 17 - (line 26) - Fluidizing Apparatus 27 - (line
28) -
Final Product 29, (ii) First Mixer 13 - (line 16) - Second Mixer 17 - (line
20) - Third
Mixer 21-(line 24) - Fluidizing Apparatus 27 - (line 28) - Final Product 29,
but also
include (iii) First Mixer 17 - (line 16') - Third Mixer 21 - (tine 24) -
Fluidizing
Apparatus 27 - (line 28) - Final Product 29, (iv) First Mixer 13 - (line 16') -
Third
Mixer 21 - (line 23) - Second Mixer 17 - (line 26) - Fluidizing Apparatus 27 -
(line
28) ~- Final Product 29, and (v) First Mixer 13 - (line 16") - Fluidizing
Apparatus
27 - (line 28) - Final Product 29.
Starting Detergent Materials
The total amount of the surfactants in products made by the present
CA 02267424 2002-O1-28
-12-
invention, which are included in the following detergent materials, finely
atomized
liquid and adjunct detergent ingredients is generally from about 5% to about
60%,
more preferably from about 12% to about 40%, more preferably, from about 15 to
about 35%, in percentage ranges. The surfactants which are included in the
above can be from any part of the process of the present invention, e.g., from
either one of the first step, the second step and/or the third step of the
present
invention.
The proposed invention is also useful in view of industrial requirement,
because the person skilled in the art can set a series of apparatuses (e.g.,
shown
in the FIG. 3) in a plant, and by using divertors which are capable for
connecting/disconnecting between each apparatus, so that the skilled in the
art
can select variations of the process to meet desired property (e.g., particle
size,
density, formula design) of the final product. Such variations include not
only the
process of the present inventions, i.e., shown as in the FIG. 3, (i) First
Mixer 13-
(line 16~-Second Mixer 17-(line 26}-Fluidizing Apparatus 27-(line 28~-Final
Product 29, (ii) First Mixer 13-(line 16~Second Mixer 17-(line 20)-Third
Mixer 21-(line 24~Fluidizing Apparatus 27-(line 28)-Final Product 29, but
also include (iii) First Mixer 17-(line 16'~Third Mixer 21-(line 24~--
Fluidizing
Apparatus 27-(line 28~Final Product 29, (iv) First Mixer 13-(line 16'x-Third
Mixer 21-(line 23~Second Mixer 17-(line 26~-Fluidizing Apparatus 27-(line
28}-Final Product 29, and (v) First Mixer 13-(line 16")-Fluidizing Apparatus
27-(line 28}-Final Product 29.
Detergent Surfactant (Agueous/Non-agueous)
The amount of the surfactant of the present process can be from about 5%
to about 60%, more preferably from about 12% to about 40%, more preferably,
from about 15 to about 35%, in total amount of the final product obtained by
the
process of the present invention.
The surfactant of the present process, which is used as the above
mentioned starting detergent materials in the first step, is in the form of
powdered,
pasted or liquid raw materials.
The surfactant itself is preferably selected from anionic, nonionic,
zwitterionic, ampholytic and cationic classes and compatible mixtures thereof.
Detergent surfactants useful herein are described in U.S. Patent 3,664,961,
CA 02267424 2002-O1-28
-12a-
Norris, issued May 23, 1972, and in U.S. Patent 3,929,678, Laughlin et al.,
issued
December 30, 1975. Useful cationic surfactants also include those described in
U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Patent
4,239,659, Murphy, issued December 16, 1980. Of the surfactants, anionics and
nonionics are preferred and anionics are most preferred.
Nonlimiting examples of the preferred anionic surfactants useful in the
present invention include the conventional C»-Cps alkyl benzene sulfonates
("LAS°), primary, branched-chain and random C,o-C2o alkyl sulfates
("AS"), the
C~o-C~8 secondary (2,3) alkyl sulfates of the formula CH3(CH2)X(CHOS03 M+)CH3
and CHs(CH2)y(CHOS03 M+)CHZCH3 where x and (y + 1 ) are integers of at least
about 7, preferably at least about 9, and M is a water-solubilizing cation,
especially sodium, unsaturated sulfates such as oleyl sulfate, and the Coo-Cps
alkyl alkoxy sulfates (°AExS°; especially EO 1-7 ethoxy
sulfates).
Useful anionic surfactants also include water-soluble salts of 2-acyloxy-
alkane-1-sulfonic acids containing from about 2 to 9 carbon atoms in the acyl
CA 02267424 2002-O1-28
group and from about 9 to about 23 carbon atoms in the atkane moiety; water
soluble salts of olefin sulfonates containing from about 12 to 24 carbon
atoms;
and beta-alkyloxy alkane sulfonates containing from about 1 to 3 carbon atoms
in the alkyl group and from about 8 to 20 carbon atoms in the alkane moiety .
Optionally, other exemplary surfactants useful in the paste of the invention
include C10-C1g alkyl alkoxy carboxylates (especially the EO 1-5
ethoxycarboxylates), the C 10-18 9lY~roi ethers, the C 10-C 1 g alkyl
poiyglycosides and the corresponding sulfated polygtycosides, and C12-C18
alpha-sulfonated fatty acid esters. If desired, the conventionat nonionic and
amphoteric surfactants such as the C12-C1g alkyl ethoxylates ("AE's including
the so-called narrow peaked alkyl ethoxylates and Cg-C12 alkyl phenol
alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C1p-C18 amine
oxides, and the like, can also be included in the overall compositions. The
C1p-
C18 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples
include the C ~ 2-C 1 g N-methytglucamides. See WO 92/06154. Other sugar
derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such
as
C10-C1g N-(3-methoxypropyl) gtucamide. The N-propyl through N-hexyl C12-
C1g glucamides can be used for low sudsing. C10-C20 conventional soaps may
also be used. If high sudsing is desired, the branched-chain C10-C1g soaps
may be used. Mixtures of anionic and nonionic surfactants are especially
useful.
Other conventional useful surfactants are listed in standard texts.
Cationic surfactants can also be used as a detergent surfactant herein
and suitable quaternary ammonium surfactants are selected from mono Cg-Clg,
preferably Cg-C10 N-alkyl or alkenyl ammonium surfactants wherein remaining N
positions are substituted by methyl, hydroxyethyt or hydroxypropyl groups.
Amphotytic surfactants can also be used as a detergent surfactant herein,
which
include aliphatic derivatives of heterocyclic secondary and tertiary amines;
zwitterionic surfactants which include derivatives of aliphatic quaternary
ammonium, phosphonium and sulfonium compounds; water-soluble salts of
esters of alpha-sulfonated fatty acids; alkyl ether sulfates; water-soluble
salts of
olefin suifonates; beta-alkyloxy alkane sulfonates; betaines having the
formula
R(R1 )2N+R2C00-, wherein R is a Cg-C 1 g hydrocarbyl group, preferably a C1 p-
C1g alkyl group or C1p-C1g acylamido alkyl group, each R1 is typically C1-C3
alkyl, preferably methyl and R2 is a C1-C5 hydrocarbyl group, preferably a C1-
G3 alkylene group, more preferably a C1-C2 alkylene group. Examples of
CA 02267424 1999-03-31
WO 98/14558 PCT/LIS97109796
-14-
suitable betaines include coconut acylamidopropyldimethy! betaine; hexadecyi
dimethyl betaine; C12-14 acylamidopropylbetaine; Cg_'4 acylamidohexyldiethyl
betaine; 4[C14-16 acylmethylamidodiethylammonio)-1-carboxybutane; C16-18
acylamidodimethylbetaine; C12-16 acylamidopentanediethylbetaine; and
[C12-16 acylmethylamidodimethylbetaine. Preferred betaines are C12-18
dimethyl-ammonio hexanoate and the C10-18 acyiamidopropane (or ethane)
dimethyl (or diethyl) betaines; and the sultaines having the formula
(R(R1}2N+R2S03- wherein R is a C6-C1g hydrocarbyl group, preferably a C10-
C16 alkyl group, more preferably a C12-C13 alkyl group, each R1 is typically
C1-
C3 alkyl, preferably methyl, and R2 is a C1-C6 hydrocarbyl group, preferably a
C1-C3 alkylene or, preferably, hydroxyalkylene group. Examples of suitable
suitaines include C12-C14 dimethylammonio-2-hydroxypropyl sulfonate, C12-
C14 amido propyl ammonio-2-hydroxypropyl sultaine, C12-C14
dihydroxyethylammonio propane suifonate, and C16-18 dimethylammonio
hexane suifonate, with C12-14 amido propyl ammonio-2-hydroxypropyl sultaine
being preferred.
Fine Powder
The amount of the fine powder of the present process, which is used in
the first step, can be from about 94% to 30%, preferably from 86% to 54%, in
total amount of starting material for the first step . The starting frne
powder of the
present process preferably selected from the group consisting of ground soda
ash, powdered sodium tripolyphosphate (STPP), hydrated tripolyphosphate,
ground sodium sulphates, aluminosilicates, crystalline layered silicates,
nitrilotriacetates (NTA), phosphates, precipitated silicates, polymers,
carbonates,
citrates, powdered surfactants (such as powdered alkane sulfonic acids) and
internal recycle sUeam of powder occurring from the process of the present
invention, wherein the average diameter of the powder is from 0.7 to 500
microns, preferably from 1 to 300 microns, more preferably from 5 to 100
microns. In the case of using hydrated STPP as the fine powder of the present
invention, STPP which is hydrated to a level of not less than 50% is
preferable.
The aluminosilicate ion exchange materials used herein as a detergent builder
preferably have both a high calcium ion exchange capacity and a high exchange
rate. Without intending to be limited by theory, it is believed that such high
calcium ion exchange rate and capacity are a function of several interrelated
factors which derive from the method by which the aluminosilicate ion exchange
CA 02267424 2002-O1-28
material is produced. In that regard, the afuminosilicate ion exchange
materials
used herein are preferably produced in accordance with Corkill et al, U.S.
Patent
No. 4,605,509 (Procter & Gamble).
Preferably, the aluminosilicate ton exchange material is in "sodium" form
since the potassium and hydrogen forms of the instant aluminosilicate do not
exhibit as high of an exchange rate and capacity as provided by the sodium
form. Additionally, the aluminosilicate ion exchange material preferably is in
over
dried form so as to facilitate production of crisp detergent agglomerates as
described herein. The aluminositicate ion exchange materials used herein
preferably have particle size diameters which optimize their effectiveness as
detergent builders. The term "particle size diameter" as used herein
represents
the average particle size diameter of a given aluminosilicate ion exchange
material as determined by conventional analytical techniques, such as
microscopic determination and scanning electron microscope (SEM). The
preferred particle size diameter of the aluminosilicate is from about 0.1
micron to
about 10 microns, more preferably from about 0.5 microns to about 9 microns.
Most preferably, the particle size diameter is from about 1 microns to about 8
microns. '
Preferably, the aluminosilicate ion exchange material has the formula
Nazj(A102)Z.(Si02)y]xH20
wherein z and y are integers of at least 6, the molar ratio of z to y is from
about 1
to about 5 and x is from about 10 to about 264. More preferably, the
aluminosilicate has the formula
Nal2j(~02)12~(Si02)121xH20
wherein x is from about 20 to about 30, preferably about 27. These preferred
aluminosilicates are available commercially, for example under designations
Zeolite A, Zeolite B and Zeoiite X. Alternatively, naturally-occurring or
synthetically derived aluminosilicate ion exchange materials suitable for use
herein can be made as described in Krummel et al, U.S. Patent No. 3,985,669.
The aiuminosilicates used herein are further characterized by their ion
exchange capacity which is at least about 200 mg equivalent of CaCOg
hardnesslgram, calculated on an anhydrous basis, and which is preferably in a
range from about 300 to 352 mg equivalent of CaC03 hardnesslgram.
CA 02267424 2002-O1-28
Additionally, the instant aluminosilicate ion exchange materials are still
further
characterized by their calcium ion exchange rate which is at least about 2
grains
Ca++/gallonlminuteJ-gramlgallon, and more preferably in a range from about 2
grains Ca++/galloNminute!-gramJgailon to about fi grains Ca++Igallonlminute!
-gramlgallon.
FinelYAtomized Liauid
The amount of the finely atomized Liquid of the present process can be
from about 1 °r6 to about 1096 (active basis), preferably from
2°~ to about 6%
(active basis) in total amount of the final product obtained by the process of
the
present invention. The finely atomized liquid of the present process can be
selected from the group consisting of liquid silicate, anionic or cationic
surfactants which are in liquid form, aqueous or non-aqueous polymer
solutions,
water and mixtures thereof. The aqueous or non-aqueous polymer solution is
dispersed
with the surfactant in step (a). Other optional examples for the finely
atomized liquid of the
present invention can be sodium carboxy methyl cellulose solution,
polyethylene glycol
(PEG), and solutions of dimethylene triamine pentamethyl phosphonic acid
(DETMP).
The preferable examples of the anionic surfactant solutions which can be
used as the finely atomized liquid in the present inventions are about 88 -
97%
active HLAS, about 30 - 50% active NaLAS, about 28°lo active AE3S
solution,
about 40-50% active liquid silicate, and so on.
Cationic surfactants can also be used as finely atomized liquid herein
and suitable quaternary ammonium surfactants are selected from mono Cg-Clg,
preferably Cg-C1p N-alkyl or alkenyl ammonium surfactants wherein remaining N
positions are substituted by methyl, hydroxyethyi or hydroxypropyi groups.
z5 Preferable examples of the aqueous or non-aqueous polymer solutions
which can be used as the finely atomized liquid in the present inventions are
modified poiyamines which comprise a polyamine backbone corresponding to
the formula:
t~-~ ~-~ ~-I~-~-~
having a modified polyamine formula V(n+1)WmYnZ or a
polyamine backbone corresponding to the formula:
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WO 98/14558 PCT/US97/09796
_17_
~E"~_~t~'k+fi'It~t' F~rr1-
~rt'~ ~k-~
having a modified polyamine formula V(n_k+1)WmYnY~kZ, wherein
k is less than or equal to n, said polyamine backbone prior to
modification has a molecular weight greater than about 200
daltons, wherein
i) V units are terminal units having the formula:
~X
E-N--('~- or E-N~ f~ or ~-N-R
to '
ii) W units are backbone units having the formula:
E X-
- ~ ~ or -N~ E'~- or
iii) Y units are branching units having the formula:
E X- O
or -N~ F~-- or -~ -F~-
and
iv) Z units are terminal units having the formula:
X-
-N-E or
E
wherein backbone (inking R units are selected from the group consisting of C2-
C12 alkylene, C4-C12 alkenylene, C3-C12 hydroxyalkylene, C4-C12 dihydroxy-
a(kylene, Cg-C12 dialkylarylene, -(R10)XR1-, -(R10)XR5(OR1)x-,
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WO 98/14558 PCT/US97/09796
_18_
-(CH2CH(OR2)CH20)z(R1 O)yR1 (OCH2CH(OR2)CH2)w-,
-C(O)(R4)rC{O)-, -CH2CH(OR2)CH2-, and mixtures thereof; wherein R1 is C2-
Cg alkylene and mixtures thereof; R2 is hydrogen, -(R10)xB, and mixtures
thereof; R3 is C1-C1g alkyl, C7-C12 arylalkyl, C7-C12 alkyl substituted aryl,
Cg-
C12 aryl, and mixtures thereof; R4 is C1-C12 alkylene, C4-C12 alkenyiene, Cg-
C12 arylalkylene, Cg-C10 arylene, and mixtures thereof; R5 is C1-C12 alkylene,
C3-C12 hydroxyalkyiene, C4-C12 dihydroxy-alkylene, Cg-C12 dialkylarylene,
-C(O)-, -C(O)NHR6NHC(O)-, -R1(OR1)-, -C(O)(R4)rC(O)-, -CH2CH(OH)CH2-,
-CH2CH{OH)CH20(R10)yR10CH2CH(OH)CH2-, and mixtures thereof; R6 is
C2-C12 alkylene or Cg-C12 arylene; E units are selected from the group
consisting of hydrogen, C1-C22 alkyl, C3-C22 alkenyl, C7-C22 arylalkyl, C2-C22
hydroxyalkyl, -(CH2)pC02M, -{CH2)qS03M, -CH(CH2COZM)COZM,
-(CH2)pP03M, -(R10)xB, -C(O)R3, and mixtures thereof; oxide; B is hydrogen,
C1-Cg alkyl, -(CH2)qS03M, -(CH2)pC02M, -(CH2)q(CHSOgM)CH2SOgM,
-(CH2)q-(CHS02M)CH2S03M, -(CH2)pP03M, -P03M, and mixtures thereof; M
is hydrogen or a water soluble cation in sufficient amount to satisfy charge
balance; X is a water soluble anion; m has the value from 4 to about 400; n
has
the value from 0 to about 200; p has the value from 1 to fi, q has the value
from
0 to 6; r has the value of 0 or 1; w has the value 0 or 1; x has the value
from 1 to
100; y has the value from 0 to 100; z has the value 0 or 1. One example of the
most preferred poiyethyleneimines would be a polyethyleneimine having a
molecular weight of 1800 which is further modified by ethoxylation to a degree
of
approximately 7 ethyleneoxy residues per nitrogen (PEI 1800, E7). It is
preferable for the above polymer solution to be pre-complex with anionic
surfactant such as NaI.AS.
Other preferable examples of the aqueous or non-aqueous polymer
solutions which can be used as the finely atomized liquid in the present
invention
are polymeric polycarboxylate dispersants which can be prepared by
polymerizing or copolymerizing suitable unsaturated monomers, preferably in
their acid form. Unsaturated monomeric acids that can be polymerized to form
suitable polymeric polycarboxylates include acrylic acid, malefic acid (or
maieic
anhydride), fumaric acid, itaconic acid, aconitic acid, mesaconic acid,
citraconic
acid and methylenemalonic acid. The presence in the polymeric
polycarboxyiates herein of monomeric segments, containing no carboxylate
radicals such as vinylmethyl ether, styrene, ethylene, etc. is suitable
provided
CA 02267424 2002-O1-28
that such segments do not constitute more than about 40% by weight of the
polymer.
Homo-polymeric polycarboxyiates which have molecular weights above
4000, such as described next are preferred. Particularly suitable homo
polymeric polycarboxylates can be derived from acrylic acid. Such acrylic acid
based polymers which are useful herein are the water-soluble salts of
polymerized acrylic acid. The average molecular weight of such polymers in the
acid form preferably ranges from above 4,000 to 10,000, preferably from above
4,000 to 7,000, and most preferably from above 4,000 to 5,000. Water-soluble
salts of such acrylic acid polymers can include, for example, the alkali
metal,
ammonium and substituted ammonium salts.
Co-polymeric polycarboxylates such as a Acrylidmaleic-based
copolymers may also be used. Such materials include the water soluble salts of
copolymers of acrylic acid and maieic acid. The average molecular weight of
such copolymers in the acid form preferably ranges from about 2,000 to
100,000,
more preferably from about 5;000 to 75,000, most preferably from about 7,000
to
65,000. The ratio of acrylate to maleate segments in such copolymers will
generally range from about 30:1 to about 1:1, more preferably from about 10:1
to
2:1. Water-soluble salts of such acrylic acidlmaleic acid copolymers can
include,
for example, the alkali metal, ammonium and substituted ammonium salts. !t is
preferable for the above polymer solution to be pre-complexed with anionic
surfactant such as LAS .
Adjunct Deterqent Ingredients
The starting detergent material in the present process can include
additional detergent ingredients and/or, any number of additional ingredients
can
be incorporated in the detergent composition during subsequent steps of the
presertt process. These adjunct ingredients include other detergency builders,
bleaches, bleach activators, suds boosters or suds suppressors, antitamish and
anticorrosion agents, soil suspending agents, soil release agents, germicides,
pH
adjusting agents, non-builder alkalinity sources, cheiating agents, smectite
clays,
enzymes, enzyme-stabilizing agents and perfumes. See U.S. Patent 3,936,537,
issued February 3, 1978 to Baskerville, Jr, et al.
Other builders can be generally selected from the various water-soluble,
alkali metal, ammonium or substituted ammonium phosphates, polyphosphates,
CA 02267424 2002-O1-28
-20-
phosphonates, polyphosphonates, carbonates, borates, polyhydroxy suifonates,
polyacetates, carboxyiates, and poiycarboxylates. Preferred are the alkali
metal,
especially sodium, salts of the above. Preferred for use herein are the
phosphates, carbonates, C1p.18 fatty acids, polycarboxylates, and mixtures
S thereof. More preferred are sodium tripolyphosphate, tetrasodium
pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof
(see below).
In comparison with amorphous sodium silicates, crystalline layered
sodium silicates exhibit a clearly increased calcium and magnesium ion
exchange capacity. In addition, the layered sodium silicates prefer magnesium
ions over calcium ions, a feature necessary to insure that substantially all
of the
"hardness" is removed from the wash water. These crystalline layered sodium
silicates, however, are generally more expensive than amorphous silicates as
well as other builders. Accordingly, in order to provide an economically
feasible
laundry detergent, the proportion of crystalline layered sodium silicates used
must be determined judiciously. Such crystalline layered sodium silicates are
discussed in Corkill et al, U.S. Patent No. 4,605,509.
Specific examples of inorganic phosphate builders are sodium and
.potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a
degree of polymerization of from about 6 to 21, and orthophosphates. Examples
of polyphosphonate builders are the sodium and potassium salts of ethylene
diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-1,
1-diphosphonic acid and the sodium and potassium salts of ethane,
1,1,2-triphosphonic acid. Other phosphorus builder compounds are disclosed in
U.S. Patents 3,159,581; 3,213,030; 3,422,021; 3.422,137; 3,400,176 and
3,400,148.
Examples of nonphosphorus, inorganic builders are tetraborate
decahydrate and silicates having a weight ratio of Si02 to alkali metal oxide
of
from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4.
Water soluble, nonphosphorus organic builders useful herein include the
various
alkali metal, ammonium and substituted ammonium poiyacetates, carboxylates,
polycarboxylates and polyhydroxy sulfonates. Examples of polyaoetate and
polycarboxylate builders are the sodium, potassium, lithium, ammonium and
substituted ammonium salts of ethylene diamine tetraacetic acid,
nitrilotriacetic
CA 02267424 2002-O1-28
-21-
acid, oxydisuccinic acid, mellitic acid, benzene potycarboxylic acids, and
citric
acid.
Polymeric polycarboxylate builders are set forth in
U.S. Patent 3,308,067, Diehl, issued March 7, 1967. Such
materials include the water soluble salts of homo- and
copolymers of aliphatic carboxylic acids such as malefic acid, itaconic acid,
mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylene
malonic acid. Some of these materials are useful as the water soluble anionic
polymer as hereinafter described, but only if in intimate admixture with the
non-soap anionic surfactant.
Other suitable polycarboxyiates for use herein are the polyacetai
carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to
Crutchfield et al, and U.S. Patent 4,246,495, issued
March 27, 1979 to Crutchfield et al. These
1 S polyacetal carboxylates can be prepared by bringing together under
polymerization condition an ester of glyoxylic acid and a polymerization
initiator.
The resulting polyacetal carboxylate ester is then attached to chemically
stable
end groups to stabilize the polyacetal carboxylate against rapid
depolymerization
in alkaline solution, converted to the corresponding salt, and added to a
detergent composition. Particularly preferred polycarboxylate builders are the
ether carboxylate builder compositions comprising a combination of tartrate
monosuccinate and tartrate disuccinate described in U.S. Patent 4,663,071,
Bush et al., issued May 5, 1987.
Bleaching agents and activators are described in U.S. Patent 4,412,934,
Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman,
issued November 20, 1984. Chelating agents are also
described in U.S. Patent 4,663,071, Bush et al., from
Column 17, line 54 through Column 18, line 68. Suds modifiers
are also optional ingredients and are described in
U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta et al., and
4,136,045, issued January 23, 1979 to Gault et al.
Suitable smectite clays for use herein are described in U.S. Patent
4,762,645, Tucker et al, issued August 9, 1988, Column 6, fine 3 through
CA 02267424 2002-O1-28
-22-
Column 7, line 24. Suitable additional detergency builders for
use herein are enumerated in the Baskerville patent,
Column 13, line 54 through Column 16, line 16, and in U.S. Patent 4,663,071,
Bush et al, issued May 5, 1987.
Octional Process Sten$
Optionally, the process can comprise the step of spraying an additional
binder in one or more than one of the first, second and/or the third mixers
for the
present invention. A binder is added for purposes of enhancing agglomeration
by providing a "binding" or "sticking" agent for the detergent components. The
binder is preferably selected from the group consisting of water, anion
surfactants, nonionic surfactants, liquid silicates, polyethylene glycol,
polyvinyl
pyrrolidone polyacrylates, citric acid and mixtures thereof. Other suitable
binder
materials including those listed herein are described in Beerse et al, U.S.
Patent
No. 5,108,646 (Procter & Gamble Co.).
Other optional steps contemplated by the present process include
screening the oversized detergent agglomerates in a screening apparatus which
can take a variety of forms including but not limited to conventional screens
chosen for the desired particle size of the finished detergent product. Other
optional steps include conditioning of the detergent agglomerates by
subjecting
the agglomerates to additional drying by way of apparatus discussed
previously.
Another optional step of the instant process entails finishing the resulting
detergent agglomerates by a variety of processes including spraying and/or
admixing other conventional detergent ingredients. For example, the finishing
step encompasses spraying perfumes, brighteners and enzymes onto the
finished agglomerates to provide a more complete detergent composition. Such
techniques and ingredients are well known in the art.
Another optional step in the process involves surfactant paste structuring
process, e.g., hardening an aqueous anionic surfactant paste by incorporating
a
paste-hardening material by using an extruder, prior to the process of the
present invention. The details of the surfactant paste structuring process are
disclosed in CA 2,268,057.
CA 02267424 2002-O1-28
-23-
In order to make the present invention more readily understood, reference
is made to the following examples, which are intended to be illustrative only
and
not intended to be limiting in scope.
EXAMPLES
~xamnle 1:
The following is an example for obtaining agglomMrates having high
density, using LSdige CB mixer (CB-30), followed by Schugi FX-160 Mixer, then
LBdige KM mixer (KM-600), and fastty using Fluid Bed Apparatus for further
granulations.
(Step 1] 250 - 270 kg/hr of aqueous coconut fatty alcohol sulfate
surfactant paste (C12-Clg, 71.5°~ active) is dispersed by the pin tools
of a CB-
30 mixer along with 220 kglhr of powdered STPP (mean particle size of 40 - 75
microns), 160 - 200 kglhr of ground soda ash (mean particle size of 15
microns),
80- 120 kglhr of ground sodium sulfate (mean particle size of 15 microns), and
the 200 kglhr of internal recycle stream of powder. The surfactant paste is
fed at
about 40 to 52°C, and the powders are fed at room temperature. The
condition
of the C8-30 mixer is as follows:
Mean residence time : 10-18 seconds
Tip speed : 7.5 -14 m/s
Energy condition : 0.5 -4 kjlkg
Mixer speed : 550 - 900 rpm
Jacket temperature : 30°C
Step 2 (i)] The agglomerates from the C8-30 mixer are fed to the Schugi
FX-160 mixer. 30 kg/hr of HLAS (an acid precursor of C11-C18 alkyl benzene
sulfonate; 94 - 97°lo active) is dispersed as finely atomized liquid in
the Schugi
mixer at about 50 to 60°C. 20-80 kg/hr of soda ash (mean particle size
of about
10 - 20 microns) is added in the Schugi mixer. The condition of the Schugi
mixer
is as follows:
Mean residence time : 0.2 - 5 seconds
Tip speed : 16 - 28 mls
Energy condition : 0.15 - 2 kjlkg
Mixer speed : 2000 ~ 3200 rpm
(Step 2 (ii)] The agglomerates from the Schugi mixer are fed to the KM-
600 mixer for further agglomeration, rounding and growth of agglomerates. 30
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PCTIUS97/09796
WO 98/14558
-24- _
kg/hr of Zeoiite is also added in the KM mixer. Choppers for the KM mixer can
be used to reduce the amount of oversized agglomerates. The condition of the
KM mixer is as follows:
Mean residence time : 3- 6 minutes
S Energy condition : 0.15 - 2 kjlkg
Mixer speed : 100 - 150 rpm
Jacket temperature: 30 - 40°C
[Step 3] The agglomerates from the KM mixer are fed to a fluid bed drying
apparatus for drying, rounding and growth of agglomerates. 20 - 80 kglhr of
liquid silicate (43% solids, 2.0 R) can be also added in the fluid bed drying
apparatus at 35°C. The condition of the fluid bed drying apparatus is
as follows:
Mean residence time : 2 - 4 minutes
Depth of unfluidized bed : 200 mm
Droplet spray size : less than 50 micron
Spray height: 175 - 250 mm (above distributor plate)
Fluidizing velocity : 0.4 - 0.8 m/s
Bed temperature : 40 - 70 °C]
The resulting granules from the step 3 has a density of about 700 g/1, and can
be
optionally subjected to the optional process of cooling, sizing and/or
grinding.
Example 2:
The following is an example for obtaining agglomerates having high
density, using L~idige CB mixer (CB-30), followed by Schugi FX-160 Mixer, then
Lbdige KM mixer (KM-600), and lastly using Fluid Bed Apparatus for further
granulations.
[Step 1] 15 kg/hr - 30kg/hr of HLAS (an acid precursor of C11-C1g alkyl
benzene sulfonate; 95% active) at about 50 °C, and 250 - 270 kg/hr of
aqueous
coconut fatty alcohol sulfate surfactant paste (C12-Clg, 71.5% active) is
dispersed by the pin tools of a CB=30 mixer along with 220 kglhr of powdered
STPP (mean particle size of 40 - 75 microns), 160 - 200 kg/hr of ground soda
ash (mean particle size of 15 microns), 80- 120 kglhr of ground sodium sulfate
(mean particle size of 15 microns), and the 200 kg/hr of internal recycle
stream
of powder. The surfactant paste is fed at about 40 to 52°C, and the
powders are
fed at room temperature. The condition of the CB-30 mixer is as follows:
Mean residence time : 10 - 18 seconds
Tip speed : 7.5 - 14 mls
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-25-
Energy condition : 0.5 - 4 kj/kg
Mixer speed : 550 - 900 rpm
Jacket temperature : 30°C
[Step 2 (i)] The agglomerates from the CB-30 mixer are fed to the Schugi
FX-160 mixer. 35 kg/hr of neutralized AE3S liquid (28% active) is dispersed as
finely atomized liquid in the Schugi mixer at about 30-40°C. 20-80
kg/hr of soda
ash is added in the Schugi mixer. The condition of the Schugi mixer is as
follows:
Mean residence time : 0.2 - 5 seconds
Tip speed : 16 - 26 m/s
Energy condition : 0.15 -2 kj/kg
Mixer speed : 2000 - 3200 rpm
[Step 2 (ii)] The agglomerates from the Schugi mixer are fed to the KM-
600 mixer for further agglomeration, rounding and growth of aggtomerates. 60
kg/hr of ground soda ash (mean particle size of 15 microns) is also added in
the
KM mixer. Choppers for the KM mixer can be used to reduce the amount of
oversized agglomerates. The condition of the KM mixer is as follows:
Mean residence time : 3- 6 minutes
Energy condition : 0.15 - 2 kj/kg
Mixer speed : 100 - 150 rpm
Jacket temperature: 30 - 40°C
[Step 3] The agglomerates from the KM mixer are fed to a fluid bed drying
apparatus for drying, rounding and growth of agglomerates. 20 - 80 kg/hr of
liquid silicate (43% solids, 2.0 R) can be also added in the fluid bed drying
apparatus at 35°C. The condition of the fluid bed drying apparatus is
as follows:
Mean residence time : 2- 4 minutes
Depth of unfluidized bed : 200 mm
Droplet spray size : less than 50 micron
Spray height: 175 - 250 mm (above distributor plate)
Fluidizing velocity : 0.4 - 0.8 m/s
Bed temperature : 40 - 70 °C
The resultant from the fluid bed drying apparatus is fed to a fluid bed
cooling
apparatus. The condition of the fluid bed cooling apparatus is as follows:
Mean residence time : 2- 4 minutes
Depth of unfluidized bed : 200 mm
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-2&
Fluidizing velocity : 0.4 - 0.8 m/s
Bed temperature : 12 - 60 °C]
The resulting granules from the step 3 has a density of about 700 g/1, and can
be
optionally subjected to the optional process of sizing an/or grinding.
Exam~~le 3:
The following is an example for obtaining agglomerates having high
density, using Lodige CB mixer (CB-30), followed by Schugi FX-160 Mixer,
further followed by using Fluid Bed Apparatus for further agglomerations.
[Step 1 J 250 - 270 kg/hr of aqueous coconut fatty alcohol sulfate
surfactant paste (C 12-C1 g, 71.5% active) is dispersed by the pin tools of a
CB
30 mixer along with 220 kg/hr of powdered STPP (mean particle size of 40 - 75
microns), 160 - 200 kglhr of ground soda ash (mean particle size of 15
microns),
80- 120 kg/hr of ground sodium sulfate (mean particle size of 15 microns), and
the 200 kg/hr of internal recycle stream of powder. The surfactant paste is
fed at
about 40 to 52°C, and the powders are fed at room temperature. The
condition
of the CB-30 mixer is as follows:
Mean residence time : 10-18 seconds
Tip speed : 7.5 - 14 m/s
Energy condition : 0.5 - 4 kj/kg
Mixer speed : 550 - 900 rpm
Jacket temperature : 30°C
[Step 2 (i)) The agglomerates from the CB-30 mixer are fed to the Schugi
FX-160 mixer. 30 kg/hr of HLAS (an acid precursor of C11-C1g alkyl benzene
sulfonate; 94 - 97% active) is dispersed as finely atomized liquid in the
Schugi
mixer at about 50 to 60°C. 20-80 kg/hr of soda ash is added in the
Schugi mixer.
The condition of the Schugi mixer is as follows:
Mean residence time : 0.2 - 5 seconds
Tip speed : 16 - 26 m/s
Energy condition : 0.15 - 2 kj/kg
Mixer speed : 2000 - 3200 rpm
[Step 3] The agglomerates from the Schugi mixer are fed to a fluid bed
drying apparatus for drying, rounding and growth of agglomerates. 20 - 80
kg/hr
of liquid silicate (43% solids, 2.0 R) can be also added in the fluid bed
drying
apparatus at 35°C. The condition of the fluid bed drying apparatus is
as follows:
Mean residence time : 2- 4 minutes
CA 02267424 1999-03-31
WO 98/14558 PCT/US97/09796
-27-
Depth of unfluidized bed : 200 mm
Droplet spray size : less than 50 micron
Spray height: 175 - 250 mm (above distributor plate)
Fluidizing velocity : 0.4 - 0.8 m/s
S Bed temperature : 40 - 70 °C
The resulting granules from the step 3 has a density of about 600 g/1 and, can
be
optionally subjected to the optional process of cooling, sizing an/or
grinding.
Having thus described the invention in detail, it will be obvious to those
skilled in the art that various changes may be made without departing from the
scope of the invention and the invention is not to be considered limited to
what is
described in the specification.
