CA1056687A - Process for the manufacture of a dishwashing detergent - Google Patents

Process for the manufacture of a dishwashing detergent

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Publication number
CA1056687A
CA1056687A CA249,812A CA249812A CA1056687A CA 1056687 A CA1056687 A CA 1056687A CA 249812 A CA249812 A CA 249812A CA 1056687 A CA1056687 A CA 1056687A
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CA
Canada
Prior art keywords
aqueous solution
agglomerate
volume
constituents
vessel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CA249,812A
Other languages
French (fr)
Inventor
Michael D. Mitchell
Gunter H. Berk
John K. Irvine
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CONN CHEM Ltd
Original Assignee
CONN CHEM Ltd
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Filing date
Publication date
Application filed by CONN CHEM Ltd filed Critical CONN CHEM Ltd
Priority to CA249,812A priority Critical patent/CA1056687A/en
Application granted granted Critical
Publication of CA1056687A publication Critical patent/CA1056687A/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/395Bleaching agents
    • C11D3/3958Bleaching agents combined with phosphates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/06Phosphates, including polyphosphates

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

A B S T R A C T

A process for the manufacture of a dishwashing detergent, containing sodium tripolyphosphate hexahydrate, in-cluding the steps of:

(a) uniformly distributing an aqueous solution of alkaline detergent salt onto a mixture of constituents, including the sodium tripolyphosphate mixing in a mixing vessel of predetermined volume to uniformly coat the constituents and essentially hydrate the sodium tripolyphosphate, the ratio of the volume of the dry constituents charged into the mixing vessel prior to the distribution of the aqueous solution of alkaline detergent salt, to the volume of the air in the vessel being between about 1:25 and 1:8;

-and-(b) mixing the formed agglomerate in the vessel to ventilate it for a predetermined time to the air of the vessel.

Description

~ ~f56f~ii87 F IE LD OF I NVE N TI ON
This invention relates to an improved process for the manufacture of dishwashing detergents in agglomerate form.
.
- BACKGROUND OF THE INVENTION
The preferred form of today's dishwashing detergents is the agglomerate because of its slower rate of solution than powders in the dishwasher, thereby prolonging the cleaning action of the detergent throughout the timed dishwashing cycle. ~?
.
Such dishwashing detergents include amoung their aotive ~onstit-` 10 uents, a source of chlorine for enhanced cleaning action, and an ?: alkaline condensed phosphate and alkaline detergent salt for ~`
.i .
~ dispersion and peptization of the dirt and soil on the dishes. ~ ~
.,. , - . ~ . .
' Where alkaline detergent salt is comprised of liquid silicates, '~.! the liquid silicates act as the binder for the source o~ chlorine, ?,~ I5 alkaline condensed phosphate and other dry ingredients in the .j j . .
,.`f agglomerate.
A typical dishwashing agglomerate includes sodium tri-~;'f polyphosphate as the alkaline condensed phosphate, sodium silicate added in solution as the alkaline detergent salt and 20 binder, and chlorinated trisodium phosphate as the source of chlorine in amounts of between 40%-50%, 30~-35~6, and 20%-30 ~ respectively. A typical agglomerate is set out below.
'~ f CONSTITUENT ~ BY WEICHT
~, . .. .
~ Sodium Tripolphosphate 42.4 ; 3 25 Chlorinated Trisodium Phosphate 21. 2 ~"
~ Sodium Silicate [ 2.4: lSi02/Na20 ] 12.2S
; Sodium Silicate [3.25: 1Si02~Na20 ] 19.00 . :f .1f Pluronic [ L 62D] * 2.00 ;~
Pluronic [ L 61 ~ * 1.00 30 Water 2.15 "f ` lOO . 00 ", -1- ~ ; ~:' . j. . .

*The pluronics are used as a source of non-ionic sur-factant polyols which may be replaced with other forms of low foam non-ionic detergents.
The chlorinated trisodium phosphate is particularly desirable since it imparts to -the detergent a good buffer capacity at high alkalinity levels during the wash cycle and per-mits effectual sheeting action during the rinse cycle to prevent water spots and streaks.
Insofar as the use of the liquid silicates is concerned, it is desirable to have an SiO2:Na20 ratio, as great as possible, for greater scrubbing action by the SiO2 and greater protection by the colloidal silica of the patterns and overglazes of fine china against erosion, while at the same time, not too great, so as to deleteriously prolong the drying time of the formulated agglomerate, which is caused by having too much SiO2. Therefore, a delicate balance must be maintained to obtain maximum benefits from the SiO2 added.
-I It is also desirable to limit the amount of Na20 in the detergent because it is a major contributor to the causticity of the detergent and erodes the glaze of fine china.
; Where sodium tripolyphosphate is used, it must be in .:, ~ its hydrated forml i.e. sodium tripolyphosphate hexahydrate, in -. the finished detergent product to be useful, so as not to hydrate in the dishwasher during the wash cycle and thereby gum, gel or cake in the dishwashing detergent dispenser, clogging same.
Therefore, such hydration must take place either prior to the sodium tripolyphosphate being incorporated into the detergent ` formulation or during the detergent's formulation. If hydrated prior to incorporation, the premanufactured sodium tripolyphos-phate hexahydrate increases the cost of the formulation. If the : , ,:~,, .
..... . . . .. , , ~ . . . . . ~ . .. . . .

i6~37 sodium tripolyphosphate is hydra-ted af-ter incorporation into the formulation, as was usually the method employed in the prior art formulations, the agglomerate "balled", forming large amorphous~
lumps containing up to about 15~ of the formulated agglomerate, and to be useful, required crushing.
While the prior art has proposed the controlling of the water content of the formulation within cer~ain limits to minimize the "balling" and formulation o the large amorphous lumps, this method has not been successful.
~ 10 It is therefore, an object of this invention to provide ~-an improved process for the manufacture of a free flowing, more uniformly agglomerated dishwashing detergent, utilizing sodium . tripolyphosphate, whereby the amount of "balling" is reduced to less than about 2%. .
Further and other objects, advantages and features of ~:
... .
the invention will be realized by those skilled in the art from the ollowing summary of the invention and detailed description : thereof.
., : ,.
SUMMAR~ OF rmE INVENTION
According to one aspect of the invention, an improved process or the agglomerating of a dishwashing detergent containing sodium tripolyphosphate hexahydrate is provided, in~

~ ! cluding the step of~

.~ (a) uniformly distributing an aqueous solution of ~ ~-..~
`; 25 alkaline detergent salt onto a mixture of .. l .
:1 constituents including sodium tripolyphosphate, being mixed in a mixing vessel of predetermined volume, to uniformly coat the constituents and essentially hydrate the sodium tripolyphosphate, j 30 the ratio of the volume of the dry constituents :: -3-.
charged into the mixing vessel prior to the distribution of the aqueous solution of al~aline detergent salt thereon, to the volume of air in ; the vessel, being between 1:2~ and about 1O8;
-and-(b) mixing the formed agglomerate in the vessel to ventilate it to the air of the vessel.
According to another aspect of the invention, an improved process for the agglomeration of a dishwashing detergent, including sodium tripolyphosphate hexahydrate is provided, in~
cluding the steps of: ~:
(a) charging dry constituents including sodium tripoly- ~ ;
' phosphate, which are to form part of the finished ayglomerate into a mixing vessel of predetermined :. .
volume for the dry mixing of same~ the ratio of . the volume of the dry constituents charged into the :
.~ mixing vessel, to the air in the vessel, being :
:~ between about 1:25 and about 1:8; ~.
.
(b) distributing an aqueous solution of alkaline detergent salt, having an SiO2/Na20 ratio of : :
between 2.4:1 and about 3.25:1, uniformly on the mixture so as to evenly coat the constituents and ~ essentially hydrate the sodium tripolyphosphate, - : subsequently addin~ sufficient water if necessary to complete the hydration; .` ~
~ (c) ventilating the agglomerate produc~; and : ; .
J (d~ subsequently sizing and aging the finished product.
-~ According to another aspect of the invention, a small amount of water may be distributed uniformly onto the mixing ; 30 dry ingredients, prior to the addition of the aqueous solution of : 4 :, 5~ 37 alkaline detergent salt to commence the hydration of the sodium tripolyphosphate.
According to another aspect of the invention, the ~ ;
i vessel of predetermined volume may comprise a horizontally dis-posed mixing drum, ro~ated about its horizontal axis, during the agglomerating process.
According to another aspect of the invention, the formed agglomerate may be aged for at least about 12 hours.
Preferably, the alkaline detergent salt is a sodium silicate.
Preferably the volume of the dry ingredient to air ratio is between about 1:18 and about 1:8. ~;
It is preferable that, where a rotating mixing drum is used, it be disposed horiæontally and the water and alkaline detergent salt be uniformly sprayed onto the mixture through a , plurali-ty of nozzles, directed generally downwardly and disposed ;~
in spaced relation on an inlet, disposed on the horizontal axis ; --of the drum. ~
... .
~l Insofar as the volume ratio between the dry constituents and air in the vessel is concerned, the larger the ratio, the greater , the amount of aeration that takes place, thus removing the need for ~ further drying techniques. However, if the ratio is much more than about 1:25, a satisfactory product is not produced. Above this ratio, there is a physical limitation on the size of the ;
mixer available today for use in the formulation of large batches.

~ With smaller batches employing a known mixing vessel, with a :' :.
ratlo of much more than about 1:25, the ability to spray the liquid components is greatly impaired. Insufficient powder surface is presented to the spray of the liquid for uniform coat-ing with the result that essentially, the wall of the clrum is ....

,,..... .: ~;.. ... . : -coated. ~ 7 If the ratio is much less than about 1:8, a greater number of large moist amorphous lumps -tend to be produced and the formulation does not benefit from sufficient aeration to preclu~de the necessity for additional drying techniques.

Theoretically to completely hydrate the sodium tri-polyphosphate used in the typical formulations, an amount of water e~ual to between about 9.2~ and about 11.5% of the formulation must be added. This water generally comes from the aqueous solution of alkaline detergent salts.
While this invention reduces "balling" substantially, still some lumps do result. However, they are both minimal in size and number and may be crushed according to known procedures.

..
DETAILED DESCRIPTION OF A PREFERRED PRO OESS OF THE INVENTION
.. . .
In the description of such preferred process, reference will be made to the schematic drawings, which illustrate the various steps of such process in diagrammatic form.
Since the percentage composition of the components of ~ the agglomerates form no part of this invention, they will not '";`! be referred to in the description of the steps of such process.
Exemplary percentages or amounts of the constituents in tested formulations manufactured according to such process are listed ;` in the examples following.

; In carrying out such preferred process, a modified Struthers-Wells mixer was used consisting of a hoxizontally 1; disposed rotatable stainless steel drum, a motor to rotate ;:J the drum about its longitudinally disposed horizontal axis, flight bars located on the inner wall of the drum for mixing in~redients charged into the drum, a station~ary longitudinally extending liquid inlet situtate on the axis of , ~ .

.
. .

rotation of the drum, a plurality of spray nozzles secured to the : inlet in spaced rela-tion and directed downwardly for the uniform ; spraying of a liquid onto the components previously charged into the drum for the uniform coating thereof.
For grinding and granulating the agglomerate formed according to such preferred process, a Sto~es granulator was employed having a fixed steel mesh screen and a plurality of steel mesh screen engaging fingers for alternately recipxocally rotating clockwise and counterclockwise through an arc of a . 10 circle to force feed the agglomerate through the steel mesh screen.
., .
PREFERRED PROCESS
.:, . .
. I With reerence to the schematic drawings, anhydrous sodium tripolyphosphate [Na5P3010] and the source of chlorine, chlorinated trisodium phosphate [4 (Na3P04.11 H20) NaOCl ] in produced Eorm, were charged inbo the rotating Struthers-Wells .~ . mixer l, shown in Schematic a through pivotable hopper 2 and .
.~ rotated to thoroughly mix these constituents. ~ ~
... .
II As the mixer continued to rotate:
(a) a small amount of water was sprayed onto the dry .~ material mixture through the nozzles of the inlet ., ~: to commence the hydration of the sodium tripoly-phosphate, seen in Schematic b;
. ~ .
.~?l (b) an a~ueous solution of alkaline detergent salt was ::i uniformly sprayed onto the rotating material for :?
.-:j the uniform coating thereof, seen in Schematic c;
(c) non-ionic surfactant polyols or other low foam non-:.., ionic detergents in solution were added -to the ~ rotating ingredients, seen in Schematic d;
:' 30 . (d) an aqueous solution of alkaline detergent salt was .

., .

668'7 ~ ~
again uniformly sprayed onto the rotating material for the uniform coating thereof, seem in Schematic e;
-and-(e) a small amount of water was sprayed onto the mix-; ing ingredients to complete the hydration of the , sodium tripolyphosphate and c:lean the inlet and spray nozzles of the highly v:iscous alkaline detergent salt solution, seen in Schematic f.

III The drum was rotated for a predetermined time after the last addition for the ventilation of the agglomerate, seen in .. . . .
Schematic g.
IV The formed agglomerate was then discharged from the `' mixer by means of hopper 2 pivoted into position for discharge into the Stokes granulator for force feeding by the fingers through the steel mesh screen, seen in Schematic h.
V The agglomerate was then sized according to size, seen in Schematic i.
(a) the oversized material, larger than 10 mesh was returned to the mixer for reprocessing as a per ! cent of the initial sodium tripolyphosphate to be `1 added;
(b) ti) the agglomerate of the desired size ( between 10 mesh and 60 mesh)~was withdrawn;
; 25 (iij subsequently aged for at least 12 hours in fiber drums at room temperature and pressure, See Schematic j ;
(iii) and packaged by methods known in the art;

` (c) the undersized, smaller than 60 mesh, was return-ed to the mixing drum for reprocessing as a per-~ centage of the sodium tripolyphosphate to be added.
; -8- -~
:.

~ ~35~137 : ~
The following ingredients comprising the indicated agglomerated dishwashing detergent were charged into the mixing drum at the indica~ed ~e accordinq to the ~referred ~rocess described above.
EXAMPLE A
.
6,000 pounds of agglomerated dishwasher detergent were manufactur- -` ed according to the above process. ,~
.
STEPS ING~EiDIENTSAMQUNT STEPS ~--Correspond to (~bs.) PERFORhMD ~ -steps outlined ELAPSED ~-in Preferred TIME
Process (Nearest Minute) I Anhydrous Sodium Tri~
polyphosphate 2544 0 .~ .
Chlorinated Trisodium $ Phosphate 1272 15 .. . .
Ratio Of Volume Of Dry i Constituents /Volume Of Air in Mixing Ves~el 1:18 Mixed 24 II (a) Water 43 27 (b) Sodium Silicate SiO2/Na20 2.4:1 735 28 `, 20 Sodium Silicate ' SiO2/Na20 3.25:1 600 52 ~ (c) Pluronics - L62D 120 ) 68 -~ ~Together~ - L61 60 ) c (d) Sodium Silicate i SiO2/Na20 3.25:1 - 540 78 ., .
(e) Water 86 93 $ 25 III Ventilation of Agglomer~
ate 95 IV Discharged 155 , V Aged : About 24 Hours.

. :
EXAMPLE B
12,000 pounds of agglomerated dishwasher detergent were manufactur-ed according to the above process.

.. _ 9 _ . . , r ~, .

~ ~5~l37 STEPS INGREDIENTS AMOUNT STEPS
Correspond To (lbs.) PERFORMED:
Steps Outlined ELAPSED
in Preferred (Neare~st Process Mlnute ) .
I Anhydrous Sodium Tri-5088 0 - 5 polyphosphate Chlorinated Trisodium Phosphate 2544 30 Ratio of Volume of Dry Constituents:Volume of Air in Mixing Vessel-1:18 Mixed 48 ; 10 II (a) Water 74 53 - (b) Sodium Silicate ~ ;
Si02/Na20 2.4:1 1470 55 ' Sodium Silicate '! Si02/Na20 3.25:1 1200 103 (c) Pluronics L62D 240 136 (d) Sodium Silicate
2/Na2 3.25:1 1080 156 (e) Water 184 185 III Ventilation of Agglomerate 190 IV Discharged 310 20 V Aged : About 24 Hours.
` Samples were taken of the agglomerated dishwashing detergents of Examples A and B, after Step III was carried out, and tested with the following results.
, FORMULATION
EXAMPLE A EXAMPLE B
~ Available Chlorine 0.69 ~ 0.61 ,,,....................................................................... : .

~i Total Actives 2.80 % 2.81 %
.~
Moisture Content 26.4 % 22.8 %
Bulk Density 0.92 gm/cc 0.87 gm/cc pH of 1% Solution 10.8 10.85 ~ ~
' ' -10- ~ :.
.: ~
. 1 .

56&j~37 Screen Analysis on 10 mesh screens 1.4 % 0.3 ~ ', through 60 mesh Screens 11.9 % 10.3 ~ , ,,, 5 Samples of other aggomerated dishwashing detergen~.s ~ manufactured according to such process were taken after Step V
', (b) (i) and samples were tested at intervals for moisture and ~ chlorine content. These samples were then aged 24 hours and again ' ~' ~ ~ .
tested for chlorine content.

ELAPSED TIMEMOISTURE CONTENT (%) CHLORINF(~) CHLORINE
-^ ~Minutes)After 24 Hours (%) ~.~
'~, 0 27.18 .83 .81 ' `'I ,:
,10 22.45 .68 .69 ~ .
`~ 15 20 ' 24.3 .71 .75 25.9 .79 .77 . ~ ~
,~ 40 26.6 ' .71 ' .72 '~
~ 50 24.6 .71 .71 ~;~
.,j , . .
'i' 60 25.2 .68 ' .66 ,~ 20 Because the manufacturing process is an aggIomeration process, the results are not uniform, due to the non-uniform ., distribution of the ingredients in the agglomerate. However, the ,~
above results show that the chlorinated ~,risodium ~hos-~ phate does not degradate. Furthermore, there was caking in the "''' samples tested prior to aging. However, after the agglomerate ~ was aged, no caking of the cons:tituents was observed.
'~ Samples of the aged agglomerate were packaged and -~ stored for twenty-four hours (Step V(b) (iii)), four boxes were '~;, opened and the dishwashing detergent was tested for moisture and chlorine content. The agglomerate from these boxes had not .::j , ~ ' ~

:~ll ' '' lCi S~137 caked and 10wed freely when poured.
: PACXAGED MATERIAL FROM SAMPLE ~:
:
BOX MOISTURE ( %)CHLORINE ( ~ ) 1 26.3 .71 :~
2 26.0 .71
3 26.1 . 73 `
4 24.4 .67 ' The extent of hydration of the sodium tripolyphosphate in the samples, based upon the amount of hexahydrate present, was determined for each box by X-ray diffraction measurements. The samples were compared to a sample containing 30~ sodium tripoly-phosphate, 50% sodium tripolyphosphate hexahydrate and 20%
chlorinated tripolyphosphate. The results are set out below.
BOX % HEXAHYDRATE OF FINAL AGGLOMERATE

1 48.5 :~
,, ~ 2 56.0 ~-~
,2 3 56.0 :, , ?~ 4 53.0 . .
As a result of the above tests, it was determined that '. 20 substantial hydration of the anhydrous sodium tripolyphosphate used in the samples had taken place.
-1 As a final test, packages of detergent manufactured ; according to such preferred process were given to various house- ~;
-i holds for use in their dishwashers and the comments of the members `
f the households were requested. All commented favourably on the product.
As many changes could be made in carrying out the j invention without departing from the scope thereof, it is intended :~2 that all matter contained within the description of such , .

preferred process and the general comments related thereto shall
5~6~37 be interpreted as illustrative of the invention and should not be ', interpreted in a limiting sense.

; ~ .'.
', : ' ~ 5 . :
," ~ ~ ~

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.~: 15 ::

.' 20 :
~.::1 ,', .'`d :'',' ' , :
j 25 . ~ ~
:,~ :

,~ . : ,~:
;- ~ . ~ .
: ~

:,, . :
`~ 30 , ~ .
,1

Claims (36)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE PROPERTY
OR PRIVILEGE IS CLAIMED ARE:
:
1. An improved process for the agglomerating of a dish-washing detergent, containing sodium tripolyphosphate hexahydrate, including the steps of:
(a) uniformly distributing an aqueous solution of alkaline detergent salt onto a mixture of con-stituents, including the sodium tripolyphosphate, mixing in a mixing vessel of predetermined volume to uniformly coat the constituents and essentially hydrate the sodium tripolyphosphate, the ratio of the volume of the dry constituents charged into the mixing vessel prior to the distribution of the aqueous solution of alkaline detergent salt, to the volume of the air in the vessel being between about 1:25 and about 1:8;
-and-(b) mixing the formed agglomerate in the vessel to ventilate it for a predetermined time to the air of the vessel.
2. The process of Claim 1, wherein the ratio of the volume of the dry constituents to the volume of air in the vessel is between about 1:18 and about 1:8.
3. The process of Claim 2, wherein the aqueous solution of the alkaline detergent salt has an SiO2/Na2O ratio of between about 2.4:1 and about 3.25:1.
4. The process of Claim 2, wherein a small amount of water is uniformly distributed onto the mixture of constituents prior to the uniform distribution of the aqueous solution of alkaline detergent salt to commence the hydration of the sodium tripoly-phosphate.
5. The process of Claim 4, wherein a small amount of water is distributed onto the constituents subsequent to the addition of the aqueous solution of alkaline detergent salt.
6. The process of Claim 3, wherein said alkaline detergent salt comprises an aqueous solution of sodium silicate.
7. The process of Claim 3, wherein an aqueous solution of a non-ionic surfactant polyol is uniformly distributed on the constituents subsequent to the uniform distribution of the aqueous solution of alkaline detergent salt.
8. The process of Claim 3, wherein an aqueous solution of a non-ionic surfactant polyol is added and the aqueous solution of alkaline detergent salt is added in two portions, one portion prior to the addition of the non-ionic surfactant polyol and the other subsequent thereto.
9. The process of Claim 8, wherein the alkaline detergent salt is an aqueous solution of sodium silicate.
10. The process of Claim 4, further including the steps of granulating the ventilated agglomerate, and conducting the granulated agglomerate to a sizing operation to obtain fractions of desirable size and undesirable size, and aging the fraction of agglomerate of desired size.
11. The process of Claim 10, wherein the agglomerate is aged for at least 12 hours.
12. The process of Claim 2, wherein the amount of sodium tripolyphosphate, added, includes a portion of agglomerate of un-desirable size, resulting from the process of Claim 10.
13. The process of Claim 2, wherein the mixing vessel is a mixing drum rotatable about its horizontal axis, which drum is rotated during the agglomerating process and includes a plurality of flighting on the interior wall in spaced relation for assisting to mix the constituents.
14. An improved process for the agglomeration of a dish-washing detergent, including sodium tripolyphosphate as the alkaline condensed phosphate, including the steps of:
(a) charging dry constituents which form a part of the finished agglomerate into a mixing vessel of predetermined volume for the dry mixing of same, the ratio of the volume of the dry constituents to the volume of air in the vessel being between about 1:18 and 1:8;
(b) distributing an aqueous solution of alkaline detergent salt, having an SiO2/Na2O ratio of between about 2.4:1 and about 3.25:1, uniformly on the mixture so as to evenly coat the constituents and essentially hydrate the sodium tripolyphosphate, subsequently adding sufficient water if necessary to complete the hydration;
(c) ventilating the agglomerating product and (d) subsequently sizing and aging the finished product.
15. The process of Claim 14, wherein the ratio of the volume of the dry constituents added to the vessel to the volume of air in the vessel is between about 1:18 and about 1:8.
16. The process of Claim 15, wherein a small amount of water is uniformly distributed onto the constituents prior to the uniform distribution of the aqueous solution of the alkaline detergent salt to commence the hydration of the sodium tripoly-phosphate.
17. The process of Claim 15, wherein the alkaline detergent salt is an aqueous solution of sodium silicate.
18. The process of Claim 15, wherein an aqueous solution of a non-ionic surfactant polyol is uniformly distributed on the constituents subsequent to the uniform distribution of the alkaline detergent salt.
19. The process of Claim 15 wherein an aqueous solution of a non-ionic surfactant polyol is added and the aqueous solution of alkaline detergent salt is added in two portions, one prior to the addition of the non-ionic surfactant polyol and the other subsequent thereto.
20. The process of Claim 19, wherein the alkaline detergent salt is an aqueous solution of sodium silicate.
21. The process of claim 15, wherein the step of sizing the finished product comprises the granulating of the ventilated agglomerate and conducting the granulated agglomerate to a sizing operation and to obtain fractions of desirable size and undesirable size and the step of aging comprises the aging of the fraction of agglomerate of desirable size.
22. The process of claim 21, wherein the agglomerate is aged for at least 12 hours.
23. The process of claim 15, wherein the mixing vessel is a mixing drum rotatable about its horizontal axis which drum is rotated during the agglomerating process and includes a plurality of flighting on the interior wall in spaced relation for assisting to mix the constituents.
24. A process for manufacturing in a single mixing vessel a free-flowing granular dishwasher detergent of typical compo-nents including hydrated forms of sodium tripolyphosphate, a sodium silicate having a weight ratio of SiO2 to Na2O between approximately 2.4:1 and approximately 3.25:1, chlorinated tri-sodium phosphates, a non-ionic surfactant and their chemical equivalents; said process comprising the steps of:
i) mixing in a ventilated mixing vessel, a dry mixture of sodium tripolyphosphate and chlorinated trisodium phosphate, the ratio of the volume of said dry mixture and the volume of said vessel being between about 1:25 and 1:8;

ii) spraying an aqueous solution of selected silicate at ambient temperature onto said dry mixture while continuing the mixing to form an agglomerate of the dry mixture during hydration of said sodium tripolyphosphate;
iii) spraying onto the formed agglomerate the non-ionic surfactant at ambient temperature;
iv) coating the treated agglomerate by spraying onto it further aqueous solution of selected silicate at ambient temperature; and v) mixing the coated agglomerate in the vessel to ventilate it to the air of the vessel while discharging the coated agglomerate from such vessel.
25. A process of claim 24 wherein approximately 40% to 50% by weight of sodium tripolyphospate, 30% to 35% by weight of chlorinated trisodium phosphate and 20% to 30% by weight in total of sodium silicate are used.
26. A process of claim 25 wherein approximately 3% by weight of non-ionic surfactant is used.
27. A process of claim 24 comprising the further inter-vening steps of:
i) (a) after mixing, spraying a minor amount of water to commence hydration of said sodium tripolyphosphate; and iv) (a) after coating, spraying a minor amount of water to flush out the spraying system used to spray said silicates.
28. A process of claim 24 wherein said volume ratio is from 1:18 to 1:8.
29. An improved process for the agglomeration of a dish-washing detergent containing sodium tripolyphosphate as the alkaline condensed phosphate, including the steps of:
(a) charging the dry constituents including sodium tripolyphosphate and a chlorinated compound for enhanced cleaning action, into a horizontally disposed rotating mixing drum, having a liquid inlet disposed therein having a plurality of spray nozzles disposed thereon in spaced relation, said drum rotating about its horizontal axis and having a plurality of interior flighting on the interior wall of the drum, for admixing the added constituents, the ratio of the volume of the dry constituents to the volume of air in the vessel being between about 1:25 and about 1:8;
(b) as the drum continues to rotate, uniformly spraying:
(i) a small amount of water onto the dry mixture through the nozzles to commence the hydration of the sodium tripolyphosphate;
(ii) an aqueous solution of alkaline detergent salt onto the rotating constituents for uniform coating thereof;
(iii) an aqueous solution of non-ionic surfac-tant polyols onto the mixture;

(iv) an aqueous solution of alkaline detergent salt onto the rotating constituents for uniform coating thereof;
(v) a small amount of water onto the mixture to complete the hydration of the sodium tripolyphosphate and clean the inlet and spray nozzles of the highly viscous alkaline detergent salt;
(c) rotating the drum for a predetermined time after the last addition for the ventillation of the agglomerate to the air of the drum;
(d) discharging the formed agglomeration from the drum granulating the agglomerate, sizing the granulated agglomerate into desirable and undesir-able fractions of agglomerate and aging the desirable fraction.
30. The process of claim 29 wherein the ratio of the volume of dry constituents to the volume of air is between about 1:18 and about 1:8.
31. The process of claim 30, wherein the source of chlorine was chlorinated trisodium phosphate.
32. The process of claim 30, wherein the aging of the desirable fraction lasts for at least 12 hours.
33. The process of claim 30, wherein the alkaline detergent salt is an aqueous solution of sodium silicate.
34. The process of claim 31 wherein the ratio of the volume of the dry constituents to the volume of air is about 1:18.
35. The process of claim 31 wherein the ratio of the volume of the dry constituents to the volume of air is about 1:8.
36. The process of claim 34 or 35 wherein the desirable fraction is aged for at least 24 hours.
CA249,812A 1976-04-08 1976-04-08 Process for the manufacture of a dishwashing detergent Expired CA1056687A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0244550A2 (en) * 1986-03-10 1987-11-11 Ecolab Inc. Process for encapsulating particles and the encapsulated product of that process
EP0323659A2 (en) * 1987-12-11 1989-07-12 Unilever N.V. Method for preparing a granular detergent material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0244550A2 (en) * 1986-03-10 1987-11-11 Ecolab Inc. Process for encapsulating particles and the encapsulated product of that process
EP0244550A3 (en) * 1986-03-10 1988-09-07 Ecolab Inc. Process for encapsulating particles and the encapsulated product of that process
EP0323659A2 (en) * 1987-12-11 1989-07-12 Unilever N.V. Method for preparing a granular detergent material
EP0323659A3 (en) * 1987-12-11 1990-10-24 Unilever Nv Method for preparing a granular detergent material and granular detergent material thereby obtained

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