Particulate composition of sodium alpha olefin sulfonate and sodium silicate

A surfactant composition adapted for use as an intermediate for particulate synthetic detergent formulations. The composition comprises sodium alpha olefin sulfonate and sodium silicate. Such compositions are in a homogeneous, storage stable, free-flowing, particulate form, and characteristically are only slightly hygroscopic.

BACKGROUND OF THE INVENTION 
This invention lies in the field of particulate sodium alpha olefin 
sulfonate (Na AOS) compositions. 
There is a need in the art of synthetic detergent formulations for a 
particulate form of Na AOS whose physical characteristics would make it 
compatible with other ingredients commonly employed in synthetic detergent 
formulations (syndets). This need arises out of the circumstance that 
syndets are commonly compounded for particular end use applications, so 
that an individual syndet can vary in terms of relative percentages of 
ingredients and in terms of ingredients present. This dictates the 
flexibility of the compounder; for example, the larger the percentage of 
inert material present with a particulate Na AOS the more limited would be 
the use field in which such a diluted Na AOS can be used. Each detergent 
formulation typically contains many different components; see "Chemical 
and Process Technical Encyclopedia" pp. 345-352, McGraw Hill Book Company 
(1974). 
Specifically, in order to prepare the class of surfactants known as sodium 
alpha olefin sulfonates in such a suitable particulate form whose physical 
characteristics would make is compatible with other ingredients commonly 
employed in synthetic detergent formulations, various efforts have been 
made to dry aqueous solutions and suspensions of this class of pure 
surfactant without known commercial success. Sodium alpha olefin sulfonate 
(sometimes herein referred to as NaAOS) characteristically, upon being 
spray or drum dried in a substantially pure form, appears to 
characteristically demonstrate severe problems of thermoplasticity, 
tackiness, free flowability, insufficient flake or bead strength 
characteristics, hygroscopicity, and the like, regardless of drying 
conditions. At the present time, it does not appear generally possible to 
dry, as by drum or spray drying on a commercial scale, aqueous solutions 
or slurries of substantially pure NaAOS so as to produce a particulate 
product comprised substantially of just NaAOS which has suitable physical 
properties for commercial blending. 
Particularly when a dried, particulate form of NaAOS is to be used in 
compounding syndets, it is not necessary for such a particulate NaAOS to 
have by itself good syndet properties, such as, for example, for laundry 
use; good syndet properties can be achieved for a laundry syndet by 
subsequent compounding using technology and know-how well known in the 
art. 
The problems of preparing a particulate system rich in NaAOS are compounded 
by the fact that NaAOS is characteristically somewhat hygroscopic. Thus, 
for example, if a slurry of NaAOS is spray-dried, the product beads will 
usually slowly take up moisture from the surrounding air over a period of 
time which makes such pure NaAOS beads, which have been stored in air for 
a period of time characteristically, somewhat undesirable for use in 
formulating synthetic detergents. Moisture absorption and inherent 
thermoplasticity tend to result in agglomeration in packout, thus yielding 
a non-pourable product. In addition, spray drying of a slurry rich in 
NaAOS invariably results in severe adhesion of product on the walls of the 
drying chamber as well as in product conveying lines thus creating a 
significant yield loss in product packout, equipment fouling problems, 
and, more importantly, a potential fire hazard within the drying unit. 
Somewhat better results in producing a commercially suitable particulate 
form of NaAOS have apparently been heretofore achieved in this art at 
least experimentally by incorporating into an aqueous solution or 
suspension of NaAOS which is to be spray or drum-dried quantities of some 
other inert (from a detergent composition standpoint) material, preferably 
one which is commonly used in detergent formulations, such as sodium 
sulfate. However, to date, so far as is how known, no one has heretofore 
ever been able to produce on a commercial scale a particulate form of 
intermediate surfactant material which is rich in NaAOS, which can be 
substantially completely comprised of active (from a detergent composition 
standpoint) components, and which, still at the same time, not only has a 
combination of physical properties making such particulate form compatible 
with other particulate agents commonly available and commonly used in 
formulating synthetic detergents, but also can be used in detergent 
formulating by simple dry blending techniques to produce an innumerable 
variety of synthetic detergent compositions intended for respective 
various specific end use applications and needs. 
For example, a drum dried sodium alpha olefin sulfonate product is 
commercially available, but this product contains appreciable quantities 
of diluents, such as sodium chloride and sodium sulfate, as well as an 
additive to suppress dusting and "firm up" the flake. The presence of the 
diluents tends to limit syndet compounding applications. 
Grant U.S. Pat. No. 3,950,276 teaches a phosphate-free laundry syndet 
composition containing olefin sulfonate, sodium silicate, non-ionic 
surfactant, and carboxymethyl cellulose. The Grant teachings contain no 
suggestion of a two-component bead type intermediate composition having 
utility as an intermediate in formulating synthetic detergent 
compositions, such as phosphate-free laundry syndet compositions. 
Parke et al U.S. Pat. No. 3,759,834 convert drum dried olefin sulfonate to 
moisturized, translucent flakes through the addition thereto of water 
followed by milling. The post-adding of free water to drum dried NaAOS to 
make flakes does not teach or suggest dry, free flowing intermediate 
compositions for syndet compounding and does not solve the problem of 
providing a bead-type concentrate product suitable for multiple syndet 
compounding applications. 
BRIEF SUMMARY OF THE INVENTION 
The present discovery provides a new and very useful particulate NaAOS 
composition of two principle components which is adapted for use as an 
intermediate or concentrate in the preparation of particulate synthetic 
detergent formulations. 
Such a composition consists on a 100 weight percent basis of a homogeneous 
mixture of 
(A) from about 25 to 65 weight percent of a sodium silicate having an 
SiO.sub.2 to Na.sub.2 O weight ratio of from about 1:1 to 2.8:1, 
(B) from about 25 to 65 weight percent of a sodium alpha olefin sulfonate 
derived from at least one alpha olefin containing from 14 to 18 carbon 
atoms per molecule, 
(C) from about 0.2 to 2 weight percent of a salt selected from the group 
consisting of sodium chloride and sodium sulfate, and 
(D) from about 4 to 15 weight percent water. 
Such a composition is further characterized by 
(A) being in the physical form of a homogeneous, storage-stable, 
free-flowing group of beads, 
(B) having a hygroscopicity not greater than about 5 percent free water 
(total composition weight basis) after standing in an atmosphere of normal 
humidity, 
(C) having a particle size such that at least about 90 weight percent of 
such group particles have at least about two dimensions in the size range 
from about 0.001 to 1 millimeter, and 
(D) having a bulk density ranging from about 0.25 to 0.50 gram per 
milliliter tamped. 
For purposes of this invention, the water content of a product composition 
as above characterized can be determined by sample ignition, or by a 
combination of sample oven drying followed by ignition. Suitable and 
preferred procedures for ignition and for oven drying are hereinbelow 
described (see Examples N and O). Typically, a composition of this 
invention contains from about 0.5 to 7 weight percent free water 
(sometimes herein referred to as free moisture), and from about 4 to 8 
weight percent water of hydration, each on a 100 weight percent total 
composition basis, though variations are possible in these values. 
The sodium chloride and/or sodium sulfate present in a product composition 
is inherently derived from the commercial method used for making NaAOS and 
it is not practical at the present time to purify a starting NaAOS by 
separating therefrom such small amounts of inorganic sodium salts, 
particularly from the standpoints of cost and commercial practicality. 
Indeed, such a level of such sodium chloride and/or sodium sulfate in a 
NaAOS formulation is regarded by many workers in the detergent industry as 
being negligible. For example, many prior art publications appear to 
ignore even the presence of such quantities of inorganic sodium salts when 
indicating, for example, surfactant weight percentage present in a syndet 
formulation. For purposes of technical accuracy, the characteristic 
presence of such small amounts of inorganic sodium salts is here detailed. 
Preparation of NaAOS is well known to the prior art and does not 
constitute as such a part of the present invention. 
The term "bead" or "beads" as used herein in reference to a product 
composition of this invention has reference to small generally ball shaped 
bodies. Sometimes the beads in a product are present as granules which are 
conglomerates of loosely bound beads. Also, sometimes the beads are not 
uniformly spherical and contain imperfections owing to the method and 
exact conditions used in drying a starting suspension. Further, sometimes 
a small (under 2 weight percent on a total product weight basis 
preferably) amount of the beads fracture into smaller bodies or particles, 
depending upon circumstances. 
In accord with this invention, such a composition as detailed above is 
prepared by spray drying at a temperature ranging from about 220.degree. 
to 450.degree. F. a starting aqueous suspension (e.g., a solution or a 
slurry) comprised initially on a 100 weight percent total suspension basis 
of from about 35 to 65 weight percent total solids, and, correspondingly, 
from about 35 to 65 weight percent water. Such solids themselves comprise 
a composition as above detailed on a 100 weight percent basis. 
The product compositions of this invention are produced from such a 
starting suspension in a two-step-type process sequence comprising: (A) 
compounding of suspension, and (B) spray drying thereof. Such a process 
sequence has obvious advantages over such prior art as Parke et al (above 
cited) wherein production of flakes involves the multiplicity of 
production steps: (1) drying of silicate, (2) preparation of NaAOS slurry, 
(3) drying of NaAOS, (4) blending of dried silicate and NaAOS, (5) 
moisturizing blend (4), (6) grinding of moisturized blend, (7) 3-roll 
milling of moisturized blend, and (8) classification of milled product. 
Furthermore the physical form (beads) of a product composition makes same 
directly useful in compounding most syndets because other syndet 
components commonly available are in a bead or particle form well suited 
from a physical standpoint for blending with a product composition of this 
invention (which would not be the case if the product were in a flake 
form). 
A preferred product composition of this invention comprises from about 36 
to 54 weight percent of sodium alpha olefin sulfonate characterized as 
above (and more preferably about 42 to 47 weight percent), and from about 
54 to 36 weight percent of sodium silicate characterized as above (and 
more preferably about 48 to 43 weight percent). 
Preferably, a product composition contains a sodium silicate which has an 
SiO.sub.2 to Na.sub.2 O weight ratio of about 2.4:1. Also, the alpha 
olefin used preferably is a mixture comprising molecules each having from 
16 through 18 carbon atoms. Preferred product compositions are comprised 
of particles which have at least two dimensions each in the range from 
about 0.18 to 0.60 mm. and which have a bulk density in the range from 
about 0.35 to 0.45 grams per milliliter. 
Furthermore, preferred compositions of this invention are characterized by 
having attrition numbers preferably not greater than about 25% (and, more 
preferably, not greater than about 20%). The term "attrition numbers" has 
reference herein to material that has been first screened through a 6 mesh 
sieve, or equivalent, and subsequently subjected to the "attrition test" 
as described herein. The attrition numbers obtained for spray dried 
products are characteristically substantially lower than about 20% while 
corresponding such numbers for drum dried compositions are 
characteristically lower than about 25%. Spray dried compositions 
preferably have attrition numbers which are not greater than about 15%, 
and, more preferably, are not greater than about 5%. One presently 
preferred class of compositions is in the form of beads characterized by 
having a size such that at least about 90 weight percent thereof have a 
number of average size distribution ranging from about 0.03 to 1.5 
millimeters. 
These compositional and chemical characteristics of a product composition 
are achieved without adversely affecting desired particulate product end 
use properties, such as water solubility, pH, foaming power, and wetting 
ability. Thus, a composition of this invention characteristically has a 
water solubility in distilled or deionized water such that at least about 
10 grams of product (and preferably at least about 15 grams of product) 
are soluble in 100 milliliters of water. A very slight haze characteristic 
is present in such a product solution because of the characteristic 
behavior of sodium silicate in water solution. The pH of a water solution 
containing a concentration of a dissolved product of about 1 weight 
percent characteristically ranges from about 10.5 to 11.5 (and preferably 
about 10.7 to 11.1 pH). The foaming power of the product is 
characteristically such that an aqueous solution of about 0.1 weight 
percent by the Ross Miles foam test method demonstrates in distilled water 
a foam height of at least about 140 ml immediately, and after five minutes 
at least about 140 ml (and preferably at least about 150 ml immediately, 
and at least about 150 ml after five minutes). Similarly, the 
characteristic wetting ability of the product when in the form of a 0.1 
weight percent aqueous solution by the Draves wetting ability test in 
distilled water demonstrates a wetting time of not more than about 70 
seconds at 25.degree. C., and not more than about 30 seconds at 50.degree. 
C. (and preferably not more than about 67 seconds at 25.degree. C., and 
not more than about 28 seconds at 50.degree. C.). 
Surprisingly and unexpectedly, the two component type silicate/sulfonate 
surfactant compositions of this invention have physical and even chemical 
characteristics which appear to be unattainable with any other practical 
binary composition of NaAOS with another component of the type used in 
detergent formulations. As examples of such other components, it is noted 
that NaAOS synthetic detergent compositions sold commercially typically 
contain, in addition to NaAOS, builder(s) (most commonly condensed 
polyphosphates, such as pentasodium tripolyphosphate or sodium 
tripolyphosphate), bleach(es) (most commonly potassium 
dichloroisocyanurate, chlorinated trisodium phosphate, sodium perborate, 
or the like), corrosion inhibitors (most commonly soluble sodium silicates 
which also contributes to detergency through their added alkalinity), 
sudsing modifiers (mono- and diethanolamides of C.sub.10-16 fatty acids 
being commonly used as sudsing boosters, and C.sub.16-22 fatty acids or 
ethoxylated fatty alcohols being commonly used as sudsing depressors), 
fluorescent whitening agents (such as sulfonated triazinylstilbenes for 
cellulosic fibers), enzymes (such as those derived from fermentation 
cultures of specific strains of boccili B. subtilis and B. licheniformis), 
antiredeposition agents (such as carboxymethyl cellulose and polyvinyl 
alcohol), hydrotopes (such as sodium xylene sulfonate, or diluents (such 
as sodium sulfate). 
The silicate/sulfonate surfactant particulate compositions of this 
invention display free flowability, homogeneity, low hygroscopicity, and 
excellent storage stability. Also, such compositions are substantially not 
thermoplastic and non-tacky. Furthermore, such compositions are prepared 
from concentrated aqueous systems, which surprisingly are themselves 
homogeneous solutions, slurries or dispersions by spray (presently 
preferred) or drum drying procedures, in contrast to the comparably 
concentrated aqueous heterogeneous solutions usually characteristic of 
other binary detergent-type compositions wherein one component is NaAOS. 
In addition, and importantly, the compositions of this invention display 
complete detergent functionality which is not possible or practical with 
most other binary detergent type compositions wherein one component is 
NaAOS. 
From another aspect, the silicate/surfactant compositions of this invention 
are also surprising and unexpected. Thus, such compositions appear to have 
a water of hydration which is apparently substantially less than the water 
of hydration content of a substantially pure, dried particulate sodium 
silicate having comparable size characteristics to compositions of the 
present invention (the sodium silicate being chemically similar to that 
used as a starting material in the comparable compositions of this 
invention). The NaAOS component in effect holds onto water as free 
moisture; water is apparently not chemically bound as water of hydration 
thereto. As respects such surfactant compositions of this invention, in 
the case of the silicate component, such reduction in water of hydration 
is surprisingly achieved without loss of water solubility characteristics, 
while as respects the NaAOS component, the presence of water of hydration 
surprisingly and unexpectedly does not impair, but rather seemingly 
improves, dried product characteristics, especially as regards, for 
example, thermoplasticity and hydroscopicity, without adversely affecting 
such properties, as, for example, free flowability. In a product 
composition of this invention, there thus arguably appears to be a species 
of synergistic coaction between the sodium silicate and the NaAOS as 
respects water of hydration. Such coaction may be an important factor in 
achieving the above indicated desirable physical properties associated 
with a product composition of this invention. While total water minus free 
moisture equals water of hydration part of the "loosely held" water of 
hydration in silicate is liberated in the free water assay. 
A product composition of this invention does not, however, display 
particularly good detergent properties by itself. Thus, for example, when 
a product composition of this invention is used as a laundry syndet, it is 
found, as might be expected by one skilled in the art of synthetic 
detergents, that the cleansing power achieved is not as good as the 
cleansing power achieved by the laundry synthetic detergent composition 
described by Grant (above cited). 
The particulate surfactant compositions of this invention can be simply and 
readily dry-mixed with other dry, particulate components with similar 
physical properties. The product syndet blends have excellent, desired 
synthetic detergent properties. Thus, the present invention makes possible 
a wide variety of very useful syndets in a highly economical and efficient 
manner. 
In addition to dry compounding, a composition of this invention can be 
added to, for example, partially formulated slurries and pastes, then 
thoroughly mixed in, for example, a crutcher, and subsequently deaerated, 
and finally spray dried. Because such compositions are in a "dry" bead 
form, addition to a crutcher can reduce water requirements for slurry 
preparation with attendant improvement in spray drying rates. 
Furthermore, a composition of this invention can be used for silicate soaps 
wherein such is added, for example, to a plodder with little or no water 
to give a generally homogeneous mass which is adapted for subsequent 
extrusion into bars of soap. 
DETAILED DESCRIPTION 
Sodium silicate in the compositions of this invention performs multiple 
functions: 
(1) It disperses or helps peptize, the soil that is removed from a fabric 
being cleansed; 
(2) It aids in the prevention of soil redeposition; 
(3) It is a corrosion inhibitor for the aluminum parts employed in most 
commercial and home laundry machines; 
(4) It exhibits buffering capacity to maintain pH level; and 
(5) It helps emulsify and sponify oily and fatty soils. 
In these compositions, as those skilled in the art will appreciate, the 
ratio of SiO.sub.2 to Na.sub.2 O is such that the less the SiO.sub.2 
content, the more the Na.sub.2 O present, and the more one approaches the 
pH of caustic soda in water solution. Generally, compositions of this 
invention employ a sodium silicate whose weight ratio of SiO.sub.2 to 
Na.sub.2 O falls in the range from about 1:1 to 2.8:1, and preferably in 
the range from about 2:1 to 2.5:1. SiO.sub.2 /Na.sub.2 O ratios generally 
above 2.0/1.0 are effective for corrosion inhibition and are preferred. 
Dried sodium silicate characteristically contains a total water content 
ranging from about 17 to 24 weight percent, and preferably about 17 to 19 
weight percent. If a given sodium silicate contains smaller amounts of 
water, say, for example, from about 15 weight percent down to 0 weight 
percent water, as one goes down in the amount of water content, the 
solubility feature of the sodium silicate in water is reduced, so that, at 
about 0 weight percent water, the silicate is only soluble with difficulty 
in water, if at all, presumably because the silicate is converted into a 
siliceous, relatively insoluble material. Consequently, the water content 
in a particulate sodium silicate is relatively critical in a composition 
of this invention, and such compositions should characteristically have a 
water of hydration content in a sodium silicate particulate material which 
is at a level where desirable water solubility characteristics are certain 
to be achieved. 
Sodium alpha olefin sulfonate surfactants are biodegradable according to 
the standards established by the Soap and Detergents Association. Thus, 
NaAOS is well over 90% biodegradable by the Shake Culture and by the 
Semi-Continuous Activated Sludge test procedures adopted by such 
Association as industry standards. Conventionally, sodium alpha olefin 
sulfonate is made from an alpha olefin containing from about 14 through 18 
carbon atoms per molecule, though commonly and for reasons of commercial 
availability, alpha olefin starting materials containing from about 15 or 
16 carbon atoms to 18 carbon atoms per molecule are employed. For example, 
when using an alpha olefin feedstock containing from about 15 to 18 carbon 
atoms per molecule, the distribution of carbon atoms in the complex 
molecular mixture comprising such an alpha olefin can be about 31% 
C.sub.15, about 29% C.sub.16, about 25% C.sub.17, and about 10% C.sub.18 
(on a total 100 weight percent composition basis). Characteristically 
also, for example, when employing a mixed alpha olefin starting material 
containing from 16 to 18 carbon atoms per molecule, such mixture can 
contain about 50 weight percent C.sub.16 and about 50 weight percent 
C.sub.18 components (same total weight basis). Other molecular weight 
distributions can be employed apparently about equally satisfactorily for 
most surfactant purposes. The sodium chloride and/or sodium sulfate is 
present in a composition of this invention because these salts are 
inherently present with NaAOS owing to the methods employed commercially 
for the manufacture of NaAOS. 
Compositions of this invention, can, of course, optionally contain minor 
amounts (e.g., preferably less than about 5 weight percent in all on a 100 
weight percent total dry composition basis) of such known additive 
materials as anti-dusting agents, such as ethoxylated alkylolamides 
(available commercially under the trademark "AMIDOX L-2" from the Stepan 
Chemical Company), and the like; anti-tack or crisping agents, such as 
trisodium sulfosuccinate, a pyrogenic silica (available commercially under 
the trademark "Cab-O-Sil EH-5" from Godfrey L. Cabot Co., or under the 
trademark "Aerosil 200" from Degussa, Inc.), calcium silicate (available 
commercially under the trademark "Microcel E" from Johns Manville Co), 
silicon dioxide (commercially available as Zeosyl 110SD from J. M. Huber 
Corporation), sodium silico aluminate (commercially available as Zeolex 
23A from J. M. Huber Corporation), and the like; hydrotopes, such as 
sodium xylene sulfonate, and the like; and others, as those skilled in the 
art will appreciate, without departing from the spirit and scope of this 
invention. Also, if desired, a composition of this invention can be 
prepared so as to contain up to about 20 weight percent, and sometimes 
more, of the conventional inerts or extenders commonly employed in the 
soap and detergent industry, such as sodium sulfate, and the like. Such 
known additives and extenders, it will be understood, will be present in a 
starting slurry, solution, or dispersion in homogeneous combination with 
sodium silicate and surfactants prior to drying, as by spray or drum 
drying. 
When such a starting slurry, dispersion, or solution contains more than 
about 40 weight percent of solids on a total suspension weight basis, 
including silicate, NaAOS and sodium sulfate, it is preferred to have a 
hydrotope present in an amount as indicated above (e.g. less than about 5 
weight percent) to promote uniformity of such slurry, solution, or 
dispersion immediately before and during the drying operation, as when a 
starting slurry so being charged to a spray drier and it is desired to 
avoid curd formation and/or stratification of slurry components in pipes, 
etc. For such plant operating reasons, it is presently preferred to have 
present in a starting aqueous suspension at least about 0.5 (but less than 
about 5) weight percent (total dry composition weight basis) of sodium 
xylene sulfonate because of its hydrotope properties. 
Starting suspension compositions are prepared by any convenient procedure. 
Conveniently, a sodium silicate having a weight ratio of SiO.sub.2 to 
Na.sub.2 O in the range above indicated in prepared as an aqueous 
solution. Commonly, such solutions are available commercially, and such 
contain a concentration of suitable sodium silicate conveniently in the 
weight range of from about 42 to 48 weight percent (100 weight percent 
solution basis). Also, a NaAOS is prepared as an aqueous solution. 
Commonly, such solutions are conventionally prepared as an integral part 
of the manufacture of NaAOS, and such contain a concentration of NaAOS 
conveniently in the weight range of from about 38 to 48 weight percent 
(100 weight percent solution basis). The preparation of respective such 
starting solutions is well known to the prior art. 
Such respective starting solutions or slurries/as the case may be are 
conveniently blended together so as to produce a mixed solution or slurry 
which is characteristically completely homogeneous and wherein the 
respective quantities of NaAOS and sodium silicate are within the ranges 
above indicated for a desired composition of this invention. 
Thereafter, the mixed solution or slurry is spray dried at temperatures in 
the range above indicated which can be accomplished using operational 
conditions for spray drying equipment which are broadly known to the prior 
art. For example, such a mixed solution is delivered by high-pressure 
pump(s) to the atomizing nozzles or via low-pressure pumps to spinning 
disks or vaned rotating wheels of a spray-drying tower under a pressure of 
from about 400 to 1100 psig for nozzles or under a pressure of from about 
5 to 50 psig for spinning disks or rotating wheels. Air may also be 
injected just prior to the nozzles to aid in puffing the droplets in the 
tower. Droplets exiting from the nozzles into the top of the tower are 
puffed into granules or beads and dried by a current of hot (typically 
ranging in the neighborhood of about 400.degree. to 450.degree. F. at 
entry though lower temperatures down to about 250.degree. F. can be 
employed) air flowing through the tower (countercurrently or concurrently, 
depending upon design and operation of equipment. Spray tower sizes vary 
widely within the detergent industry. Some of the newer, high capacity 
commercial towers are as large as 25 feet in diameter and about 100 feet 
tall. 
Granules or beads exit from the bottom of the tower and are carried away 
by, for examples, conveyor belts, vibrating conveyors, gravity flow to 
storage bins, air conveying to silos, or the like. The product can be 
cooled by contact with either ambient or preconditioned air, and then 
minor ingredients, such as perfume, or the like, which are too sensitive 
to pass through the spray-drying operation, may be admixed with, or 
sprayed on, the product beads or granules. The finished beads or granules 
are then transferred by some handling system, such as a pneumatic system, 
or the like, to a silo, or to a finished product packaging line, all as 
desired. 
Typical air flow rates range from about 16,000 to 100,000 SCFM at air 
pressures ranging from about 0.7 to 1 atmosphere. Typical solids residence 
times range from about 0.5 to 10 seconds. 
Preferably, a starting suspension is preheated to a temperature in the 
range from about 150.degree. to 180.degree. F. though higher and lower 
such temperatures can, of course, be employed. 
In spray drying, water vapor is separated substantially at the rate 
produced and while maintaining the interior of the drying zone at the 
temperature preferably ranging from about 250.degree. to 350.degree. F. 
As indicated, a product composition of this invention is admixable with 
other particulate materials conventionally used in syndet compositions. 
Such other materials are commonly available commercially, and simple 
mechanical mixing procedures may be used for blending, such as baffled or 
unbaffled rotating drums, twin shell blender, plowhsare mixer (Littleford 
Lodige) or ribbon blender (Marion), auger mixer, or the like, as is well 
known in the art. 
Commercial spray drying of substantially pure NaAOS solutions is 
impractical at best for a number of specific technical reasons. For one 
thing, a dry NaAOS is extremely thermoplastic at high (substantially pure) 
active organic strength. For another thing, because of this 
thermoplasticity, such a dry product adheres to surfaces, and would adhere 
to the walls of a spray drying tower resulting in a potential fire and 
explosion hazard, among other obvious problems. For example, any product 
that did not stick on tower walls would "snowball" or agglomerate into 
"doughballs" which would plug the drier system causing an automatic 
shutdown. These problems are particularly troublesome with an NaAOS made 
with an alpha olefin mixture involving C.sub.14 to C.sub.18 alpha olefins 
and are further magnified by introduction of lower molecular weight alpha 
olefins, i.e. under C.sub.14. 
Commercial drum drying of substantially pure NaAOS solutions is likewise 
impractical at best. The product thermoplasticity causes an accumulation 
of product to develop on drier knives like "taffy candy" rather than 
coming away therefrom as sheet, flake, or powder. 
The gumming product must be hand-scraped away from knives, and the 
resulting product form has no known market. Such a NaAOS product would 
perhaps have to be cooled or frozen, and then micropulverized, at great 
equipment and processing cost; however, on attaining room temperature, the 
so-produced product would undoubtedly agglomerate, especially with NaAOS 
made with alpha olefin mixtures wherein lower carbon content (such as 
C.sub.12, C.sub.14, and C.sub.15) olefins are present in significant 
quantities. 
Sodium silicate materials of the type used in compositions of the present 
invention can, when in aqueous solution form, be spray dried to produce 
free-flowing, non-thermoplastic particulate products which are extremely 
hygroscopic.

EMBODIMENTS 
The present invention is further illustrated by reference to the following 
Examples. Those skilled in the art will appreciate that other and further 
embodiments are obvious and within the spirit and scope of this invention 
from the teachings of these present Examples taken with the accompanying 
specification. 
EXAMPLE A 
From Philadelphia Quartz Company is obtained an aqueous solution containing 
about 42 weight percent sodium silicate having an SiO.sub.2 to Na.sub.2 O 
weight ratio of about 2.4/1, (100 weight percent basis). 
EXAMPLE B 
From Philadelphia Quartz Company is obtained an aqueous solution containing 
about 48 weight percent sodium silicate having an SiO.sub.2 to Na.sub.2 0 
weight ratio of about 2.4/1, (100 weight percent basis). 
EXAMPLE C 
From Stepan Chemical Company is obtained an aqueous solution containing 
about 45.6 weight percent total dissolved solids and about 44 weight 
percent NaAOS (100 weight percent basis). The NaAOS is prepared by using 
an alpha olefin mixture in the C.sub.15 to C.sub.18 range having a carbon 
distribution (on a 100 weight percent total olefin basis) of about 31 
weight percent C.sub.15 molecules, about 29 weight percent C.sub.16 
molecules, about 25 weight percent C.sub.17 molecules, and about 10 weight 
percent C.sub.18 molecules. 
EXAMPLE D 
From Stepan Chemical Company is obtained an aqueous solution containing 
about 43.2 weight percent total dissolved solids and about 39.5 weight 
percent NaAOS (100 weight percent basis). The NaAOS is prepared by using 
an alpha olefin mixture in the C.sub.16 to C.sub.18 range having a carbon 
distribution (on a 100 weight percent total olefin basis) of about 50 
weight percent C.sub.16 molecules, and about 50 weight percent C.sub.18 
molecules. 
EXAMPLE E 
From Stepan Chemical Company is obtained an aqueous solution containing 
about 45.6 weight percent total dissolved solids and about 44 weight 
percent NaAOS (100 weight percent basis). The NaAOS is prepared by using 
an alpha olefin mixture in the C.sub.16 to C.sub.18 range having a carbon 
distribution (on a 100 weight percent total olefin basis) of about 50 
weight percent C.sub.16 molecules and about 50 weight percent C.sub.18 
molecules. 
EXAMPLE F 
For purposes of the present invention, the procedure used to determine 
"attrition number" is as follows: The fragility of the product flake is 
determined by subjecting a fixed volume of product to milling in a glass 
jar containing three rows of vertical vigreaux indentations spaced about 
120.degree. apart. The indentations or teeth serve to "rake" the product 
at least three times for each complete revolution of the jar. The ability 
of the product flake to withstand fracture during this "raking" process is 
reflected in the % Volume Loss after milling. This volume loss can be 
translated to a numerical value of "toughness" or "non-friability". Thus 
the higher the attrition number or % volume loss, the greater is the 
fragility of the product. 
Procedure for Determining Attrition Number 
The relative fragility of the screened product flake is determined using 
the following procedure: 
a. Transfer 100 ml. of tamped screened product to 1000 ml. attrition test 
jar. This jar comprises a conventional-type quart wide mouth, flat 
bottomed glass vessel containing three circumferentially spaced vertically 
extending rows of circumferentially staggered Vigreaux indentations with 6 
or 7 such indentations per row, each indentation being from about 3/8 to 
1/2 inch deep radially. 
b. Place on roller mill and mix for 20 minutes at a jar speed of 72 rpm. 
This equates to about 4320 "rakings" in the 20 minute test period. 
c. Next, transfer product from jar to 100 ml. graduate. Tamp lightly, as in 
density determination, to constant volume. Record volume. 
d. The volume of product before milling minus the volume after milling = % 
Volume Loss. The % Volume Loss is also arbitrarily referred to in this 
application as the "Attrition Number". Then: 
##EQU1## 
where V.sub.1t = tamped volume of product before milling; and 
V.sub.2t = tamped volume of product after milling. 
Thus, an "attrition number" is the percent volume loss after a milling of 
the product. 
EXAMPLE G 
For purposes of the present invention, the procedure used to determine 
"free flowability" of a particulate solid material is as follows: 
Of Free-Flowability 
Definition: 
The property of motion resulting from the freedom of the constituent 
particles to move independently of one another; the property of a type of 
motion where the cohesive forces between the same or similar substances 
are so minimal as to afford freedom of movement in pouring a given product 
from the confines of a prechosen container. 
Procedure 
This is accomplished by 
(a) noting the angle of repose assumed by the product before movement or 
flow of particles is initiated, and 
(b) observing the ease of flow of the product particles though progressive 
plastic funnels having discharge orifices of 15 mm. and 10 mm (i.d) 
respectively. 
EXAMPLE H 
For purposes of the present invention, the procedure used to determine 
"homogeneity" of a particulate solid material is as follows: 
Of Homogeneity 
Definition: 
The state of being uniform in composition and structure. 
Procedure: 
Strictly qualitative. The uniformity of a blend is determined by observing 
for (1) evidence of individual ingredients, (2) variation in particle 
size, (3) color differences between particles, and (4) classification or 
separation due to differences in particle density. 
EXAMPLE I 
For purposes of the present invention, the procedure used to determine 
"hygroscoposity" of a particulate solid material is as follows: 
Of Hygroscopicity 
Definition: 
The state of readily adsorbing and retaining moisture. 
Procedure: 
Determined qualitatively by (1) exposure of spray dried material to ambient 
conditions of high relative humidity (75%), (2) squeezing material by hand 
to form a clump, and (3) dropping the clump on a hard surface (or rubbing 
between both hands) to assess the relative ease of disintegration of 
agglomerates. 
EXAMPLE J 
For purposes of the present invention, the procedure used to determine 
"storage stability" of a particulate solid material is as follows: 
Of Storage Stability 
Definition: 
The state of being unvarying in chemical composition and physical state or 
condition. 
Procedure: 
Both qualitative and quantitative. 
(1) Samples of products are analyzed before and after prolonged (6 months) 
storage. Products of this invention showed no significant changes in 
chemical composition. 
(2) Similarly, samples of products of this invention before and after 
prolonged storage (6 months) show no significant change in tamped bulk 
density, fines, and free-flowability. 
EXAMPLE K 
For purposes of the present invention, the procedure used to determine the 
character of a starting aqueous mixture used to make a particulate solid 
product composition of this invention in terms of (a) "homogeneity" or 
"heterogeneity", and (b) true "solution" or "dispersion" is as follows: 
Definitions: 
Homogeneity: 
The state of being uniform in composition and structure; 
Heterogeneity: 
The state of being detectably dissimilar in ingredients or constituents; 
True solution: 
The condition of being completely dissolved, a liquid containing a 
dissolved substance; 
Dispersion: 
The state of fine particles distributed more or less evenly throughout a 
medium; 
Procedure: 
Strictly qualitative. The character of a starting aqueous mixture as 
defined by the foregoing terms is assessed by visual means after noting 
the consistency and condition of the mixture under static and dynamic 
conditions (i.e. at rest and under moderate to vigorous agitation). The 
aqueous mixture is observed under agitation and at rest; the latter over a 
period of 1 to 90 seconds. Observe that the maximum residence time of the 
aqueous mixture in the pumping line to a Bowen spray head is preferably 
not in excess of about 90 seconds. 
EXAMPLE L 
For purposes of the present invention, the procedure used to determine 
"thermoplasticity" of a particulate solid material is as follows: 
Of Thermoplasticity 
Definition: 
The state of being softened under heat. 
Procedure: 
A thermoplastic substance is quite rigid at normal temperatures and under 
normal conditions of stress. However, it is capable of deformation under 
heat and pressure. With the foregoing in mind, this property is assessed 
by visual observation of the product in various stages of drying. 
On a drum drier, the relative flexibility of the product sheet issuing from 
the drier knives is assessed by flexing the sheet. Thermoplastic material 
behaves like rubber, non-thermoplastic cracks like "corn flakes". 
Similarly, the brittleness of the product in the drier pans is assessed by 
chopping the flake with a spatula. Thermoplastic flakes resist breakage 
and agglomerate under this treatment. Also, there is a tendency for the 
flakes to stick to the spatula like "taffy". In contrast, 
non-thermoplastic flakes are readily fractured with no perceptible 
adhesion to drier pans or spatula. 
In spray tower operation, the product is sampled below the hopper fed by 
the cyclones and at the discharge point to the storage silos. At free 
moisture levels of 11/4% or under, compression of the product by hand to 
give a solid clump indicates that the product is thermoplastic. Failure of 
the material to respond in this manner indicates it is non-thermoplastic. 
EXAMPLE M 
For purposes of the present invention, the procedure used to determine 
"functionality" of a particulate solid product composition of this 
invention is as follows: 
Of Functionality 
Definition: 
The state of being designed or developed chiefly from the point of view of 
use. A principal utility of a product of this invention is believed to be 
in heavy-duty laundry detergents and in various industrial and 
institutional cleaners as exemplified in the exemplary formulations below: 
EXAMPLE M.1 
HEAVY-DUTY LAUNDRY SYNDET 
______________________________________ 
% by weight Mixing 
Ingredients (total wt. basis) 
Order 
______________________________________ 
Product of Example 7 (below) 
27.0 7 
BIO SOFT EA-8 5.0 5 
Sodium Tripolyphosphate (light grade) 
35.0 1 
Sodium carbonate (light grade) 
16.4 2 
Sodium Sulfate 15.3 3 
Sodium Carboxymethylcellulose 
(Hercules 6-CTL or 7LT) 
1.0 4 
Tinopal 5BM 0.15 6 
Tinopal RBS-200 0.15 6 
Colorant and Fragrance (as desired) 
q.s. 
______________________________________ 
Equipment: Rotating drum 
Compounding Procedure 
A. charge 1,2,3 and 4 to drum and mix 5 minutes. 
B. atomize 5 at about 50.degree. C onto resulting mixture, continue mixing 
until 5 has been uniformly distributed throughout dry blend. Avoid 
overmixing to prevent premature glomulation. 
C. next, add 6 and 7 followed by colorant and perfume as desired. Mix until 
a discrete particle or glomule is formed. Then discharge blender via 10 
mesh sieve to packout hopper. 
"Bio Soft EA-8" is an ethoxylated fatty alcohol nonionic surfactant 
available commercially from Stepan Chemical Company, Northfield, Illinois. 
"Tinopal 5BM" is a bis tri azinyl derivative of 4,4' diaminostilbene - 
2,2'-disulfonic acid, sodium salt available commercially from Ciba Geigy 
Corporation, Summit, New Jersey. "Tinopal RBS-200" is a 
naptho-triazostilbene sulfonate, sodium salt available commercially from 
Ciba Geigy Corporation. 
EXAMPLE M2 
TRUCK WASH 
______________________________________ 
Mixing 
Ingredient % by Wt. Order 
______________________________________ 
Product of Example 7 (below) 
35.0 4 
Sodium Sesquicarbonate 
20.0 3 
Trisodium Phosphate (dodecahydrate) 
25.0 1 
Sodium Tripolyphosphate (light granular) 
20.0 2 
Blue Colorant (FD & C Aluminum Lake) 
q.s. 5 
Fragrance q.s. 6 
100.0% 
______________________________________ 
Equipment: Twin shell blender 
Compounding Procedure: 
A. combine 1, 2, and 3; mix until uniform. 
B. incorporate the Product of Example 7, color, and fragrance into the 
formulation and mix until homogeneous. 
______________________________________ 
pH of 1% Solution: 10.5 
Density: gm/ml: 0.630 
Lbs./ft..sup.3 39.3 
______________________________________ 
EXAMPLE M.3 
WAX STRIPPER 
______________________________________ 
Mixing 
Ingredients % by Wt. Order 
______________________________________ 
Product of Example 7 (Below) 
40.0 4 
Sequestrene* NA-4 2.0 3 
Sodium Carbonate (light, granular) 
29.0 2 
Trisodium Phosphate (dodecahydrate 
granular) 29.0 1 
Colorant (FD & C Aluminum, Lake) 
q.s. 5 
Fragrance q.s. 6 
100.0% 
______________________________________ 
Equipment: Ribbon blender. 
Compounding Procedure: 
A. combine 1, 2, and 3; mix until uniform. 
B. continue the mixing and incorporate the STEPANSIL AS-50 (product of 
Ex.7) color and fragrance. Mix until homogeneous. 
______________________________________ 
pH of 1% Solution: 11.2 
Density: gm/ml: 0.590 
Lbs./ft..sup.3 36.8 
______________________________________ 
"Sequestrane NA-4" is a tetrasodium ethylendiamine tetraacetate dihydrate 
available commercially from Ciba Geigy Corporation. 
EXAMPLE M.4 
WHITEWALL TIRE CLEANER 
______________________________________ 
Mixing 
Ingredient % by Wt. Order 
______________________________________ 
Product of Example 7 (below) 
50.0 2 
Trisodium Phosphate (dodecahydrate 
granular) 50.0 1 
Fragrance q.s. 3 
100.0% 
______________________________________ 
Equipment: Plowshare mixer 
Compounding Procedure: 
A. combine ingredients and mix until uniform. 
______________________________________ 
pH of 1% Solution: 11.6 
Density: gm/ml: 0.610 
Lbs./ft..sup.3 38 
______________________________________ 
The performance of a product composition of this invention in three 
heavy-duty laundry detergents is assessed in accordance with the procedure 
detailed below: 
Initially, the following formulations are prepared: 
EXAMPLE M.5 
______________________________________ 
Mixing 
Ingredients % by wt. Order 
______________________________________ 
50/50 Silicate/Na-AOS 
(see Example 1 Below) 
30.0 7 
Sodium Tri-polyphosphate 
(Monsanto Light) 35.0 1 
Sodium Carboxy methylcellulose 
(Hercules 7LT) 2.5 2 
Tinopal 5BM 0.35 3 
Tinopal RBS-200 0.35 4 
Sodium Carbonate (Flozan) 
15.9 5 
Sodium Sulfate (Technical) 
15.9 6 
______________________________________ 
Equipment: Twin Shell Blender 
Compounding Procedure: 
A. charge 1, 2, 3, 4, 5 and 6 to blender and mix for 5 minutes. 
B. next add 7 and mix for 5 minutes. 
EXAMPLE M.6 
______________________________________ 
Mixing 
Ingredients: % by wt. Order 
______________________________________ 
50/50 Silicate/Na-AOS 
(See Example 1 below) 
24.0 7 
Bio Soft EA-8 5.0 8 
Sodium tripolyphosphate 
35.0 1 
Na.sub.2 CO.sub.3 16.4 2 
Na.sub.2 SO.sub.4 16.4 3 
CMC, Na-Salt 2.5 4 
Tinopal 5BM 0.35 5 
Tinopal RBS-200 0.35 6 
______________________________________ 
Equipment: Twin Shell Blender 
Compounding Procedure: 
A. charge 1, 2, 3, 4, 5 and 6 to a blender and mix 5 minutes. 
B. atomize 8 onto the resulting mixture and continue mixing until uniform. 
C. add 7 and mix for 5 minutes. 
EXAMPLE M.7 (Prior Art) 
Commercially available detergent: 
Tide (8.7% as Phosphorus) (Proctor & Gamble) 
Compounding procedure: Unknown 
Exact formulation: Unknown 
Procedure Summary: Detergency tests are run in tap water and 300 ppm water 
using: 
1. Spangler Sebum Soil method of evaluating detergents. 
2. Standard soiled test cloths from United States Testing and Test Fabrics. 
3. Laboratory prepared clay soiled cotton. 
Anti-Redeposition tests are run in tap water using the Lever Brothers 
method. 
Conclusions: 
1. The test products of Examples M.5 and M.6 performed equal to or better 
than the Tide of Example M.7 in cotton detergency. 
2. Tide of Example M.7 is slightly better than the test products in 
detergency on the commercially available soiled test cloths. 
3. Tide is significantly poorer than the test products in anti-redeposition 
on cotton. 
4. In overall detergency and anti-redeposition the AOS and AOS/EA-8 syndet 
outperformed the Tide of Example M.7. 
______________________________________ 
TEST CONDITIONS FOR DETERGENCY 
______________________________________ 
Machine: Terg-O-Tometer 
Agitator Speed: 90 CPM 
Detergent Concentration: 
0.15% 
Wash & Rinse Temperature: 
120.degree. F 
Wash Cycle: 15 minutes 
Rinse Cycle: 2 Hand, Tap Water 
Size of Swatches: 4 1/2" .times. 6" 
Wash Load*: 15 g./liter 
______________________________________ 
*For the Bandy Black Clay soiled cotton, this is 4 - 41/2" .times. 6" 
swatches. 
For the Sebum Soil and Clay soiled swatches each pot contained: 
2 - 41/2 inches .times. 6 inches Cotton 
2 - 41/2 inches .times. 6 inches 65/35 Polyester/Cotton Resin Treated. 
2 - 41/2 inches .times. 6 inches 65/35 Polyester Cotton with no Resin. 
______________________________________ 
TEST CONDITIONS FOR REDEPOSITION 
______________________________________ 
(Lever Brothers Test) 
Machine: Terg-O-Tometer 
Agitator Speed: 90 CPM 
Detergent Concentration: 
0.15% 
Wash & Rinse Temperature: 
120.degree. F 
Wash Cycle: 15 minutes 
Rinse Cycle: 2 - 3 minute rinses. 
Soil Load: 1.10 grams Bandy Black Clay/ 
125.degree. ml. 
Wash Load: 4 - 41/2 .times. 6" cotton swatches 
______________________________________ 
The detergent and the clay are dispersed in the pots and the swatches are 
added and washed for 15 minutes. The swatches are then machine rinsed 
twice for 3 minutes. Upon completion of the second and fifth wash/rinse 
cycles the swatches are machine dried and measured on both sides for 
reflectance using the Gardner Reflectometer with a Tri-Green filter. The 
average of eight readings is reported. The higher the reflectance reading, 
the better the anti-redeposition properties of the test product. 
TABLE 1 
______________________________________ 
DETERGENCY ON CLAY SOILED COTTON 
Tap Water 
% Reflectance 
95% 
Standard Confidence 
Detergent Average Deviation Limits 
______________________________________ 
AOS Syndet 76.01 0.865 .+-. 0.690 
AOS/EA-8 Syndet 
76.38 0.498 .+-. 0.398 
Tide 75.06 1.147 .+-. 0.916 
300 PPM Water 
AOS Syndet 74.22 1.082 .+-. 0.864 
AOS/EA-8 Syndet 
74.47 1.151 .+-. 0.919 
Tide 72.83 0.529 .+-. 0.423 
______________________________________ 
TABLE 2 
______________________________________ 
Detergency On Sebum Soil/Clay Soiled Cotton 
(300 PPM Water) 
First Cycle 
% Reflectance 
95% 
Standard Confidence 
Detergent Average Deviation Limits 
______________________________________ 
AOS Syndet 76.77 -- -- 
Tide 76.35 -- -- 
AOS/EA-8 Syndet 
76.92 -- -- 
Second Cycle 
AOS Syndet 75.67 -- -- 
Tide 75.10 -- -- 
AOS/EA-8 Syndet 
76.50 -- -- 
Third Cycle 
AOS Syndet 73.80 0.308 .+-. 0.348 
Tide 73.00 0.158 .+-. 0.179 
AOS/EA-8 Syndet 
75.47 0.369 .+-. 0.418 
______________________________________ 
TABLE 3 
______________________________________ 
Detergency On Sebum Soil/Clay 
Soiled 65/35 Polyester/Cotton With Resin Finish 
(300 PPM Water) 
First Cycle 
% Reflectance 
95% 
Standard Confidence 
Detergent Average Deviation Limits 
______________________________________ 
AOS Syndet 79.85 -- -- 
Tide 79.85 -- -- 
AOS/EA-8 Syndet 
79.27 -- -- 
Second Cycle 
AOS Syndet 79.57 -- -- 
Tide 79.90 -- -- 
AOS/EA-8 Syndet 
79.32 -- -- 
Third Cycle 
AOS Syndet 79.20 0.187 .+-. 0.211 
Tide 79.15 0.083 .+-. 0.094 
AOS/EA-8 Syndet 
79.20 0.187 .+-. 0.211 
______________________________________ 
TABLE 4 
______________________________________ 
Detergency On Sebum Soil/Clay 
Soiled 65/35 Polyester/Cotton With No Resin Finish 
(300 PPM Water) 
First Cycle 
% Reflectance 
95% 
Standard Confidence 
Detergent Average Deviation Limits 
______________________________________ 
AOS Syndet 79.80 -- -- 
Tide 79.90 -- -- 
AOS/EA-8 Syndet 
79.75 -- -- 
Second Cycle 
AOS Syndet 79.42 -- -- 
Tide 79.87 -- -- 
AOS/EA-8 Syndet 
79.77 -- -- 
Third Cycle 
AOS Syndet 78.95 0.166 .+-. 0.187 
Tide 78.85 0.050 .+-. 0.056 
AOS/EA-8 Syndet 
79.40 0.274 .+-. 0.309 
______________________________________ 
TABLE 5 
______________________________________ 
DETERGENCY DATA FOR SEBUM SOIL/CLAY 
SOILED FABRICS RUN IN TAP WATER 
Cotton Reflectance, % 
Detergent 1st Cycle 2nd Cycle 3rd Cycle 
______________________________________ 
AOS Syndet 79.90 79.17 78.82 
Tide 79.62 78.47 78.37 
AOS/EA-8 Syndet 
79.97 79.12 79.15 
65/35 Polyester/Cotton 
(Resin Finish) 
AOS Syndet 80.65 80.40 80.65 
Tide 80.07 80.32 80.67 
AOS/EA-8 Syndet 
79.60 79.97 80.07 
65/35 Polyester Cotton 
(No Resin Finish) 
AOS Syndet 80.85 80.92 80.90 
Tide 80.92 80.92 80.85 
AOS/EA-8 Syndet 
80.37 80.72 80.72 
______________________________________ 
No significant differences between formulations are shown. 
TABLE 6 
______________________________________ 
Second Cycle 
% Reflectance 
95% 
Standard Confidence 
Detergent Average Deviation Limits 
______________________________________ 
AOS Syndet Ref. 595-28 
79.27 0.916 .+-. 0.732 
AOS/EA-8 Syndet Ref. 
595-30 79.97 0.066 .+-. 0.053 
Tide 75.28 1.105 .+-. 0.883 
Fifth Cycle 
AOS Syndet 78.22 0.927 .+-. 0.741 
AOS/EA-8 Syndet 
79.55 0.255 .+-. 0.204 
Tide 72.84 0.387 .+-. 0.309 
______________________________________ 
TABLE 7 
______________________________________ 
DETERGENCY ON SOILED COTTON 
FROM TEST FABRICS AND UNITED STATES TESTING 
(Tap Water) 
Detergency Units 
(% Reflectance) 
Detergents: U.S.T. Test Fab. 
______________________________________ 
Tide 6.77 10.10 
AOS Syndet 5.57 9.05 
AOS/EA-8 Syndet 3.27 7.70 
______________________________________ 
EXAMPLE N 
For purposes of the present invention, the procedure used to determine 
"water of hydration" of a particulate solid product of this invention is 
as follows: 
"Water of hydration" is not used herein in the strictest chemical sense of 
a definite amount of water in stoichiometric proportion in combination 
with a definite chemical substance as, for example, in crystals, e.g., 
calcium chloride, CaCl.sub.2. H.sub.2 O, but is rather to be taken to mean 
the difference between the "total water content" of a particulate solid 
product of this invention and its "free moisture level" as defined in 
Example O. 
The "total water content", for the purposes of this invention, is 
determined by a procedure involving measurement of the percentage weight 
loss on ignition, termed LOI, followed by suitable mathematical 
corrections which convert by calculation said LOI to a "percent total 
water content". Total water content is meant to include free moisture, 
water of hydration, water of imbibition, and constitutional water 
(chemically bound water). 
Ignition is carried out at temperatures of 800.degree.-900.degree. C. As 
ignition of the organic components of the particulate solid product of 
this invention takes place concurrently during this procedure, it is 
necessary to apply appropriate correction factors (loss on ignition 
factors) to correct for this burning loss. Thus, it can be shown that: 
##EQU2## 
where %Surf = % surfactant solids (including salts, neutral oil, 
hydrotropes, etc.) 
f.sub.Surf = loss on ignition factor for the surfactant 
f.sub.A = loss on ignition factor for the additive 
%LOI = % loss on ignition (LOI) for total spray dried sample 
%H.sub.2 O-T = % total water 
%A = % additive 
and 
##EQU3## 
The above equation is derived from theoretical considerations of the 
ignition characteristics of the individual components, i.e. NaAOS 
surfactant sodium silicate, and additives that comprise the product of 
this invention. 
EXAMPLE O 
For purposes of the present invention, the procedure used to determine 
"free moisture level" of a particulate solid product of this invention is 
as follows: 
"Free moisture level" of a particulate solid product of this invention is 
defined as the percentage of water that it readily removed, essentially 
reversibly, by heating at 105.degree. C. for a period of 3 hours. 
The procedure involves accurately measuring the weight loss of a 1 to 2 
gram sample of particulate solid product thinly spread over the surface of 
a 70 mm. diameter crystallizing dish (or the like), heated in an oven at 
105.degree. C. for 3 hours. 
EXAMPLE P 
For purposes of the present invention the procedure used to determine "bulk 
density tamped" of a particulate solid product of this invention is as 
follows: 
The density of blends of this invention is determined on a screened product 
by filling and refilling a tared 100 ml. graduated cylinder to mark, after 
tamping on a rubber grid (10 times), until the volume remained constant at 
100 ml. The net weight of the product divided by 100 = gm/ml. 
The following Examples illustrate embodiments of the present invention: 
EXAMPLE 1 
Using portions of the solution of Example B and portions of the solution of 
Example D, a mixed homogeneous batch suspension having the following 
composition is prepared: 
______________________________________ 
Component Parts by Weight 
______________________________________ 
Sodium silicate solution 156 
NaAOS solution 189 
(Total) 345 
______________________________________ 
The starting batch is prepared in a 40 gallon open top stainless steel tank 
and is agitated until a uniform suspension results at ambient conditions. 
The resulting mixed suspension is subjected to spray drying using a 
cocurrent pilot plant spray drying tower manufactured by Bowen Engineering 
Company. The conditions of operation are as follows: 
______________________________________ 
Slurry feed rate 
(Moyno Utility pump) 
3.5 pounds/minute 
Slurry feed temp. 75-80.degree. F. 
Bowen spray head: 
Wheel dia. and type 5 inch vaned 
Disc speed 18,000 rpm 
Inlet air temp. 
(direct gas heat) 390.degree. F. 
Outlet air temp. 240.degree. F. 
______________________________________ 
The dried product removed from the bottom of the tower is in the form of 
granules or beads at least about 90 weight percent (total weight basis) 
are in the form of granules or beads having diameters in the range from 
about 0.01 to 0.1 mm. Upon analysis of the product, it is found to 
comprise (100 weight % total composition basis): 
About 41.74 weight percent sodium alpha olefin sulfonate having a 
composition as described above; 
About 41.74 weight percent of sodium silicate having a composition as 
described above; 
About 13.41 weight percent total water; 
About 1.50 weight percent sodium chloride; and 
About 1.60 weight percent sodium sulfate. 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 
about 6.57 weight percent (100 weight 
percent total composition basis) 
Bulk density tamped 
about 0.56 gram per milliliter 
Free flowability 
yes 
Thermoplasticity 
no 
Homogeneity yes 
Hygroscopicity 
no 
Storage stability 
yes 
Functionality 
100% 
Attrition number 
1.8 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. This material can be produced on commercial scale 
spray drying equipment. 
EXAMPLE 2 
Using portions of the solution of Example B and portions of the solution of 
Example D, a mixed homogeneous batch suspension slurry is prepared in a 40 
gallon open top stainless steel tank and agitated until a uniform solution 
or slurry results at ambient conditions. The active composition is as 
follows: 
______________________________________ 
Component Parts by Weight 
______________________________________ 
sodium silicate solution 156 
NaAOS solution 189 
(Total) 345 
______________________________________ 
The resulting mixed suspension is subjected to spray drying using the same 
cocurrent pilot plant spray drying tower as in Example 1. The conditions 
of operation were as follows (the solution or slurry being pumped into the 
tower top via a Moyno utility pump): 
______________________________________ 
Slurry feed temp. 75-80.degree. F. 
Slurry feed rate 3.1 lbs./min. 
Centrifugal atomizer 
Wheel dia. & type 5 inch vaned 
Wheel speed 14,000 rpm 
Air inlet temp. 
(direct gas heat) 390.degree. F. 
Air outlet temp. 240.degree. F. 
Air exhaust 2000 c.f.m. 
______________________________________ 
The dried product removed from the bottom of the tower is in the form of 
granules or beads at least 90 weight percent of which range from 0.01 to 
0.11 mm. The chemical composition (100 weight % total basis) comprises: 
______________________________________ 
NaAOS 42.14 
Sodium Silicate 42.14 
Total water 12.60 
NaCl 1.51 
Na.sub.2 SO.sub.4 
1.61 
______________________________________ 
The product composition has the following additional characteristics: 
______________________________________ 
Water of hydration 
6.54 weight percent (total composition 
basis) 
Free moisture 
6.06 weight percent (total composition 
basis) 
Bulk density tamped 
0.544 gm./ml. 
Free flowability 
yes 
Thermoplasticity 
no 
Homogeneity yes 
Hygroscopicity 
no 
Storage stability 
yes 
Functionality 
100% 
Attrition number 
1.9 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
EXAMPLE 3 
Using portions of the solution of Example B and portions of the solution of 
Example D, a mixed homogeneous batch solution is prepared in a 40 gallon 
open top stainless steel tank and agitated until a uniform suspension 
results at ambient conditions. The active composition is as follows: 
______________________________________ 
Component Parts by Weight 
______________________________________ 
sodium silicate solution 156 
NaAOS solution 189 
(Total) 345 
______________________________________ 
The resulting mixed suspension is subjected to spray drying using the same 
cocurrent pilot plant spray drying tower as in Example 1. The conditions 
of operation were as follows (the solution being pumped into the tower top 
via a Moyno utility pump): 
______________________________________ 
Slurry feed temp. 75-80.degree. F. 
Slurry feed rate 5.0 lbs./min. 
Centrifugal atomizer 
Wheel dia. & type 5 inch vaned 
Wheel speed 14,000 rpm 
Air inlet temp. 
(direct gas heat) 450.degree. F. 
Air outlet temp. 258.degree. F. 
Air exhaust 2000 c.f.m. 
______________________________________ 
The dried product removed from the bottom of the tower is in the form of 
granules at least 90 weight percent of which range from 0.020 to 0.155 
millimeters. The chemical composition (100 weight % total basis) 
comprises: 
______________________________________ 
NaAOS 42.14 
Sodium Silicate 42.14 
Total water 12.59 
NaCl 1.51 
Na.sub.2 SO.sub.4 
1.61 
______________________________________ 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 
5.68 weight percent (total composition 
basis) 
Bulk density tamped 
0.528 gm./ml. 
Free flowability 
yes 
Thermoplasticity 
no 
Homogeneity yes 
Hygroscopicity 
no 
Storage stability 
yes 
Functionality 
100% 
Attrition number 
2.0 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
EXAMPLE 4 
Using portions of the solution of Example B and portions of the solution of 
Example D, a mixed homogeneous batch solution is prepared in a 40 gallon 
open top stainless steel tank. In addition, there is added to the mixture 
molten ethoxylated alkylolamide (available commercially under the 
trademark "Amidox L-2" from Stepan Chemical Company). The resulting 
mixture is agitated until a uniform suspension results at ambient 
conditions. The composition is as follows: 
______________________________________ 
Component Parts by Weight 
______________________________________ 
Sodium silicate solution 104 
NaAOS solution 127 
Ethoxylated alkylolamide 
2.5 
(Total) 233.5 
______________________________________ 
The resulting mixture suspension is subjected to spray drying using the 
same cocurrent pilot plant spray drying tower as in Example 1. The 
conditions of operation were as follows (the suspension being pumped into 
the tower top via a Moyno utility pump): 
______________________________________ 
Slurry feed temp. 72-80.degree. F. 
Slurry feed rate 3.6 lbs./min. 
Centrifugal atomizer 
Wheel dia. & type 5 inch vaned 
Wheel speed 14,000 rpm 
Air inlet temp. 
(direct gas heat) 380.degree. F. 
Air outlet temp. 240.degree. F. 
Air exhaust 2000 c.f.m. 
______________________________________ 
The dried product removed from the bottom of the tower upon analysis is 
found to comprise (100 weight percent basis): 
______________________________________ 
NaAOS 41.78 
Sodium silicate 41.78 
Total water 12.85 
Sodium chloride 1.32 
Ethoxylated alkylolamide 0.85 
Sodium sulfate 1.42 
______________________________________ 
This product is in the form of granules at least about 90 weight percent of 
which range in size from about 0.02 to 0.165 mm. 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 5.48 wt. % (total composition) 
basis) 
Bulk density tamped 
0.510 gm/ml. 
Free flowability yes 
Thermoplasticity no 
Homogeneity yes 
Hygroscopicity no 
Storage stability 
yes 
Functionality 100% 
Attrition number about 1.5 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
EXAMPLE 5 
Using portions of the solution of Example B and portions of the solution of 
Example D, a mixed homogeneous batch suspension is prepared in a 40 gallon 
open top stainless steel rank. In addition, there is added to the mixture 
trisodium sulfosuccinate. The resulting mixture is agitated until a 
uniform suspension results at ambient conditions. The composition is as 
follows: 
______________________________________ 
Component Parts by Weight 
______________________________________ 
Sodium silicate solution 104 
NaAOS Solution 127 
Trisodium sulfosuccinate 2.5 
(Total) 233.5 
______________________________________ 
The resulting mixed suspension is subjected to spray drying using the same 
cocurrent pilot plant spray drying tower as an Example 1. The conditions 
of operation were as follows (the solution being pumped into the tower top 
via a Moyno utility pump): 
______________________________________ 
Slurry feed temp. 70-75.degree. F. 
Slurry feed rate 3.7 lbs./min. 
Centrifugal atomizer 
Wheel dia. & type 5 inch vaned 
Wheel speed 14,000 rpm 
Air inlet temp. 
(Direct gas heat) 380.degree. F. 
Air outlet temp. 246.degree. F. 
Air exhaust 2000 c.f.m. 
______________________________________ 
The dried product removed from the bottom of the tower upon analysis is 
found to comprise (100 weight percent basis): 
______________________________________ 
Sodium sulfate 1.52 
NaAOS 42.07 
Sodium silicate 42.07 
Total water 11.97 
Sodium chloride 1.42 
Trisodium sulfosuccinate 0.95 
______________________________________ 
This product is in the form of granules at least about 90 weight percent of 
which range in size from about 0.02 to 0.165 mm. 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 5.03 wt. %(total composition 
basis) 
Bulk density tamped 
0.534 gm/ml. 
Free flowability yes 
Thermoplasticity no 
Homogeneity yes 
Hygroscopicity no 
Storage stability 
yes 
Functionality 100% 
Attrition number 3.0 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
EXAMPLE 6 
Using portions of the solution of Example B and portions of the solution of 
Example E, a mixed homogeneous batch solution is prepared by first 
charging the portions of Example E solution to a tank. After the agitator 
is started, the portions of Example B solution are pumped into the tank 
and the mixture is heated to about 145.degree. to 150.degree. F. Before 
the portions of Example E solution are charged to the tank, sufficient 
sodium xylene sulfonate is charged to and dissolved in solution E to make 
this resulting solution contain 3.0 weight percent sodium xylene sulfonate 
(based on total weight of NaAOS plus sodium xylene sulfonate). The mixture 
in the tank is agitated until a uniform solution results. The composition 
is as follows: 
______________________________________ 
Parts 
Components by Weight Quantities 
______________________________________ 
Sodium silicate solution 
135.41 13,541 lbs. 
NaAOS solution with 
sodium xylene sulfonate 
147.72 14,772 lbs. 
283.13 28,313 lbs. 
______________________________________ 
The resulting mixed solution or slurry is subjected to spray drying using a 
full-scale cocurrent spray drying tower manufactured by Bowen Engineering 
Company. The conditions of operation were as follows: 
______________________________________ 
Air throughput 72,000 c.f.m. 
Slurry feed temp. 150.degree. F. 
Slurry feed rate 9500 lbs./hr. 
Slurry viscosity at 50.degree. C. 
840 cps 
Centrifugal atomization 
Wheel dia. & type 11 inch vaned. 
Wheel speed 7200 rpm 
Inlet air temp. 
(direct gas fired) 380.degree. F. 
Outlet air temp. 265.degree. F. 
Product density (tamped) 
0.38 gm/ml. 
Particle size 125 to 350 microns. 
______________________________________ 
The dried product removed from the bottom of the tower upon analysis is 
found to comprise (100 weight percent basis): 
______________________________________ 
NaAOS 42.06 
Sodium silicate 42.06 
Total water 13.79 
Sodium chloride 0.28 
Sodium xylene sulfonate 1.32 
Sodium sulfate 0.47 
______________________________________ 
This product is in the form of granules at least about 90 weight percent of 
which range in size from about 0.10 to 0.34 mm. 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 5.48 weight percent (total composition 
basis) 
Bulk density tamped 
0.38 gm./ml. 
Free flowability 
yes 
Thermoplasticity 
no 
Homogeneity yes 
Hygroscopicity 
no 
Storage stability 
yes 
Functionality 100% 
Attrition number 
2.0 
Color off white 
______________________________________ 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
EXAMPLE 7 
A 40 weight percent aqueous solution of sodium xylene sulfonate is 
prepared, and a 40 weight percent aqueous solution of sodium sulfate is 
prepared. These solutions are blended with a mixed solution of portions of 
Example A solution and portions of Example E solution prepared in the 
manner taught in Example 6. The resulting starting mixture is a 
homogeneous solution or slurry (depending upon its temperature) having the 
following composition: 
______________________________________ 
Parts by Solids or 
Component Weight Actives 
______________________________________ 
Sodium silicate solution 
160.0 67.2 
NaAOS solution 164.5 67.2 
Sodium xylene 
sulfonate solution 
4.75 1.9 
Sodium sulfate solution 
84.3 33.7 
Total Batch 413.6 
______________________________________ 
The resulting mixed suspension is subjected to spray drying using the same 
cocurrent pilot plant spray drying tower and same conditions of operation 
as in Example 1. 
The dried product removed from the bottom of the tower upon analysis is 
found to comprise (100 weight percent basis): 
______________________________________ 
NaAOS 33.65 
Sodium silicate 33.65 
Total water 12.95 
Sodium chloride 1.61 
Sodium xylene sulfonate 0.95 
Sodium sulfate 17.20 
______________________________________ 
This product is in the form of granules or beads at least about 90 weight 
percent of which range in size from about 0.02 to 0.165 mm. 
The product has the following additional characteristics: 
______________________________________ 
Free moisture 5.48 wt. % (total composition basis) 
Bulk density tamped 
0.510 gm./ml. 
Free flowability 
yes 
Thermoplasticity 
no 
Homogeneity yes 
Hygroscopicity 
no 
Storage stability 
yes 
Functionality 100% 
Attrition number 
3.0 
Color Off white 
______________________________________ 
The total water in the silicate/surfactant blends of this invention is 
preferably of the order of about 12 .sup..+-. 3 %. Thus, with "Free 
moistures" preferably running about 5 .sup..+-. 1 %, the water of 
hydration is preferably in the neighborhood of about 4 to 9%. 
The physical and chemical properties of this composition demonstrate that 
it is suitable for use as an intermediate in preparing particulate 
synthetic detergents. 
Example 1 demonstrates that spray drying can be used to prepare a product 
of this invention. Examples 2, 3 and 4 illustrate various compositional 
types and spray drying ranges within the teachings of the present 
invention. Examples 4 through 7 demonstrate that various additives can 
surprisingly be present as minor components in compositions of this 
invention without adversely interferring with desired product properties. 
Other and further objects, aims, purposes, embodiments, advantages and the 
like will be apparent to those skilled in the art from a reading of the 
present specification without departing from the spirit and scope thereof.