US2622068A - Process of making heat dried detergent compositions containing form ii sodium triphosphate - Google Patents
Process of making heat dried detergent compositions containing form ii sodium triphosphate Download PDFInfo
- Publication number
- US2622068A US2622068A US31174A US3117448A US2622068A US 2622068 A US2622068 A US 2622068A US 31174 A US31174 A US 31174A US 3117448 A US3117448 A US 3117448A US 2622068 A US2622068 A US 2622068A
- Authority
- US
- United States
- Prior art keywords
- triphosphate
- detergent
- mixture
- aging
- hydration
- 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 - Lifetime
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
- C11D3/062—Special methods concerning phosphates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/06—Inorganic compounds
- C11D9/08—Water-soluble compounds
- C11D9/10—Salts
- C11D9/14—Phosphates; Polyphosphates
Definitions
- the present invention relates to a method for the manufacture of detergent mixtures containing alkali metal triphosphates (sometimes called alkali metal tripolyphosphates), and particularly to the incorporation of slowly hydrating anhydrous triphosphates in aqueous detergent compositions.
- alkali metal triphosphates sometimes called alkali metal tripolyphosphates
- Triphosphate in finely divided form exhibit the undesirable property of forming lumps that dissolve very slowly in water even though the mixture is well stirred.
- the tendency to form lumps or agglomerates, I have found varies with the phase or form of crystalline structure of the phosphate.
- Form I finely divided triphosphates containing substantial amounts of the high temperature form, usually referred to as Form I, show a very marked tendency to lump when stirred into aqueous fluids even though the mixture is stirred vigorously.
- triphosphates of the Form II variety Prior to the present invention, however, triphosphates of the Form II variety have had the objectionable tendency, when used in the manufacture of heat dried detergent compositions, of producing powders of a sticky nature that are not free flowing and that cake badly under slight pressure in storage bins, packing machines and in packed cartons.
- sticky I refer to an objectionable tendency of the individual spray dried granules to agglomerate with one another, and compact, cake or adhere to other objects that the granules moveover or contact.
- Form II varieties in marked contrast to the Form I varieties, hydrate extremely slowly (even though they have a higher immediate solubility than the Form I varieties). This slow hydration behavior appears to be responsible for the aforementioned difiiculties heretofore encountered when Form II triphosphates have been used in making detergent compositions, doubtless because a major portion of the water in the final dried product has been present as free water rather than as water of hydration.
- the invention contemplates substantially complete hydration of Form II triphosphates in aqueous fluid detergent mixtures so as to prevent stickiness and reduce the dustiness of the dried detergent composition made therefrom.
- Figure 1 illustrates the conditions of time and temperature wherein approximately '10 per cent reversion of sodium triphosphate occurs during aging in the aqueous detergent compositions.
- Figures 2 to 5 represent X-ray diffraction patterns characteristic of four different phosphates as follows:
- Ordinary'soaps such as the alkali metal salts of the higher fatty acids that may be ob-, tained from naturally occurring plant or animal esters or that may be produced synthetically (e. g.
- Anionic detergents (excluding true soaps), such as water-soluble salts of sulfuric and phosphoric acid reaction products of alkyl and "substituted alkyl compounds containing from 8 to 18 carbon atoms in the alkyl group,
- Non-ionic detergents such as the reaction products of higher alcohols and higher fatty acids with. considerable amountsof alkylene oxides,
- phosphate in the aqueous detergent mixtures can readily be accomplished by aging, within the tem-.-. perature range of to 200 F., in a manner. adapted to prevent settling and separation of the undissolved salts.
- merous other devices e. g. screw conveyors. or long pipelines, wherein sufficient storage timeis to be had to permit substantially complete hygdration to the hexahydrate.
- Sodium triphosphate is a metastable materialin water solution. It hydrolyzes or reverts,slow-. 1y to form normal and acid salts of other, phOSf.
- Example I -38 parts of a slowly hydrating
- Form II sodium triphosphate having a part1 size such that it would pass through a, Tyle x with 58 parts of an aqueous fluid containing;
- the aging may be eflect-... ed in a vessel equipped With agitators or in nuwater and 24% of sodium alkyl sulfate prepared by sulfating the fatty alcohols obtained by the reduction of coconut oil, and 4 parts of soda ash were then added.
- the somewhat thin slurry obtained therefrom was mixed thoroughly for 20 minutes and then aged for 6 hours at 165 F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed without incorporating large amounts of air.
- Example I The marked benefit obtained through the aging process is shown by comparing the product in Example I with a product obtained by spray drying a like, aqueous, detergent-triphosphate mixture that had not been aged.
- the latter was a sticky, fragile and dusty product, the particles of which caked and lumped, and broke down badly to form more dust during the packaging operation.
- This product contained only 3% moisture.
- Another portion of the same unaged slurry that was spray dried so as to leave 9% moisture in the product gave a damp material that balled badly when handled.
- Example II --32 parts of a moderately slowly hydrating Form II sodium triphosphate, having a particle size such that it would pass through a Tyler standard 35 mesh screen, were thoroughly mixed with 48 parts of an aqueous fluid containing 60% water and 23% sodium alkyl sulfate, and 14 parts of an aqueous fluid containing 65% water and 16.4% of alkyl benzene sulfonate, to which were added 5 parts of soda ash. The somewhat thin slurry obtained therefrom was aged by slowly agitating it for a total of 4 hours at a temperature of 170 F., during which period it gradually became a viscous but yet pumpable mixture.
- Said slurry was then spray dried in well known manner yielding a highly satisfactory, rapidly dissolving, efficient detergent composition, in solid granular form, that was free flowing, comparatively dustless, non-sticky and comprised of tough granules that did not break down to any significant amount during subsequent packaging operations. Analysis showed it to contain moisture.
- Example III --36 parts of a poorly hydrating Form II sodium triphosphate were thoroughly mixed with 59 parts of an aqueous fluid containing 60% water and 24% of sodium alkyl sulfate, and 5 parts of soda ash were then added.
- the somewhat thin slurry obtained therefrom was mixed thoroughly and then aged for 5 hours at 160 F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed without incorporating large amounts of air.
- the slurry gradually became a viscous but yet pumpable mixture which was then dried as a film or thin sheet over steam heated rolls,
- the somewhat thin slurry obtained therefrom was mixed thoroughly for 20 minutes and then aged for 6 hours at F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed.
- the Form II triphosphate is a major component and was, in fact, present in greater quantity than the organic detergent.
- detergents of each of the various types enumerated in de-- fining may be substituted for the deproportion of triphosphate is used, very little of the triphosphate is in solution at any one time during the processing operations, most of t being merely suspended as a slurry.
- the triphosphate used should in general have a particle size no larger than that desired in the final product.
- This invention in its broad aspects is not restricted to the manufacture of detergent mixture'si containing in,..addition.- tootheorganicr dee. tergentonly; sodium triphosphatee but .mayalso be. applied ;in the manufacture .of 1 detergents comprising triphosphates .of potassiumand' other. alkali: metals.
- n th r qce e o manufacturing a heatdried detergent me e i n .s h ant l y reeof du t and of stickinessand caking properties the steps of incorporating Form 'I'I 'so'diunr triphosphate in a fluid detergent mixture containingnasf the .w te rsqlub ..salt of amember selected from theglfgl ll. consisting .50 ,.mi .tu'r s thereci containingfrom s to'18ca 0 atszms intheallgyl active detergent ingredient of Sulfuric t ie Pre i cts. o a k l. and s b stituted- 'allg'yl *cornpounds,
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (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)
- Detergent Compositions (AREA)
Description
Dec.
Filed June 4, 1948 16, 1952 E. s. HIZER 2,522,063
PROCESS OF MAKING HEAT DRIED DETERGENT COMPOSITIONS CONTAINING FORM 1: SODIUM TRIFHOSPHATE 2 SHEETSSHEET 1 flare fi w/z flare/#04; w UV Z655 /d% Wave/31017 All 77029 a/{yfiy I //00/5 QYWWM fife/2362132912625 Mrzejs ONS ' 16, 1952 4 E. 5. HI
- PROCESS OF MAKING HEAT DRIED DETERGENT couposrrr 2 SHEETS-SHEET 2 I CONTAINING FORM II SODIUM TRIPHOSPl-IATE Filed June 4. l9
Standard X-Ruy Patterns of Sodium 'Triand Pym-Phosphots Na P O I N0 P O 'SH O 3 m Zileri 6- 125x67 0J2, 9'- wa sm W Patented Dec. 16, 1952 PROCESS OF MAKING HEAT DRIED DETER- GENT COMPOSITIONS CONTAINING FORM II SODIUM TRIPHOSPHATE Elbert S. Hizer, Cincinnati, Ohio, assignor to The Procter and Gamble Company, Ivorydale, Ohio, a corporation of Ohio Application June 4, 1948, Serial No. 31,174
3 Claims.
The present invention relates to a method for the manufacture of detergent mixtures containing alkali metal triphosphates (sometimes called alkali metal tripolyphosphates), and particularly to the incorporation of slowly hydrating anhydrous triphosphates in aqueous detergent compositions.
Some varieties of triphosphate in finely divided form exhibit the undesirable property of forming lumps that dissolve very slowly in water even though the mixture is well stirred. The tendency to form lumps or agglomerates, I have found, varies with the phase or form of crystalline structure of the phosphate. Thus I find that finely divided triphosphates containing substantial amounts of the high temperature form, usually referred to as Form I, show a very marked tendency to lump when stirred into aqueous fluids even though the mixture is stirred vigorously. However, I have found that comparably finely divided triphosphates of the low temperature phase usually referred to as Form II, show little or no tendency to agglomerate under like conditions, and the present invention relates to the use of these Form II triphosphates in the manufacture of detergents.
Prior to the present invention, however, triphosphates of the Form II variety have had the objectionable tendency, when used in the manufacture of heat dried detergent compositions, of producing powders of a sticky nature that are not free flowing and that cake badly under slight pressure in storage bins, packing machines and in packed cartons.
In order to avoid a damp product which would lump and ball much worse, extreme atomization has been used to facilitate the spray drying of such compositions causing them to be fragile and dusty as well as sticky. 7
By sticky I refer to an objectionable tendency of the individual spray dried granules to agglomerate with one another, and compact, cake or adhere to other objects that the granules moveover or contact.
It is found that the Form II varieties, in marked contrast to the Form I varieties, hydrate extremely slowly (even though they have a higher immediate solubility than the Form I varieties!) This slow hydration behavior appears to be responsible for the aforementioned difiiculties heretofore encountered when Form II triphosphates have been used in making detergent compositions, doubtless because a major portion of the water in the final dried product has been present as free water rather than as water of hydration.
It is an object of this invention to provide a method for the manufacture of non-sticky detergent compositions using Form II triphosphates and to reduce the dustiness of said detergent compositions.
More specifically the invention contemplates substantially complete hydration of Form II triphosphates in aqueous fluid detergent mixtures so as to prevent stickiness and reduce the dustiness of the dried detergent composition made therefrom.
I have discovered that suitable aging of aqueous fluid detergent mixtures containing Form II triphosphate prior to heat drying gives the unique and unexpected result of eliminating the sticky properties otherwise obtained in the heat dried detergent composition prepared therefrom. The time and temperature conditions of this aging are critical, as will subsequently be explained.
I have also discovered that this same aging greatly reduces the dustiness of the detergent product. The starting effect of aging is shown in a product, which was made from an aqueous detergent mixture containing Form II sodium triphosphate in particulate form that was aged for 8 hours before spray drying. It was a freefiowing, hard, non-sticky, tough, granular, nondusty product that did not break down during the packaging operations. It had a dry feel even though it contained 10 per cent moisture. In direct contrast an identical batch of the same composition that was not aged before spray drying gave a sticky product that caked and lumped badly during the packaging opera-'- tion even though it contained only 3 per centmoisture. In addition the granules were dusty and so fragile that they broke down to give more dust during the packaging operation.
I have further discovered that substantially complete hydration of the sodium triphosphate .to the hexahydrate should be accomplished during the above mentioned aging period in the aqueous fluid detergent mixture.
In the accompanying illustrations Figure 1 illustrates the conditions of time and temperature wherein approximately '10 per cent reversion of sodium triphosphate occurs during aging in the aqueous detergent compositions.
Figures 2 to 5 represent X-ray diffraction patterns characteristic of four different phosphates as follows:
Figure 2, anhydrous sodium triphosphate in the phase known as Form I, V
Figure3, anhydrous sodium triphosphate in the phase known as Form II,
Figure 4, sodium triphosphate hexahydrate, and
Figure 5, anhydrous sodium pyrophosphate.
In this specification and the appended claims I employ the term detergent to designate organic detergents, including:
(1) Ordinary'soaps such as the alkali metal salts of the higher fatty acids that may be ob-, tained from naturally occurring plant or animal esters or that may be produced synthetically (e. g.
by oxidation of petroleum, or by hydrogenationof carbon monoxide by the Fischer-Tropsch proc ess) resin acids and/or naphthenicacids.
(2) Synthetic organic detergents characterized by their high solubility in water; their resistance to precipitation by the constituents of hard water,
and their surface active and efiective detergent properties, which include:
(a) Anionic detergents (excluding true soaps), such as water-soluble salts of sulfuric and phosphoric acid reaction products of alkyl and "substituted alkyl compounds containing from 8 to 18 carbon atoms in the alkyl group,
(b) Non-ionic detergents, such as the reaction products of higher alcohols and higher fatty acids with. considerable amountsof alkylene oxides,
(c) Cationic detergents, such as certain quaternary ammonium'groups and certain amine groups neutralized with acids each of which is preferably employed in its water-soluble salt form, bearing in mind, however, that some cationic detergents have but limited utility in strongly alkaline com position.'
Numerous examples of such synthetic. organic detergents are mentioned in Linds U. '8. Patent We include in the term detergent composition and/or detergent mixture, in'addition 'tdone or more of the above detergents,- alkaline builders? or detergent improving agents such as alkaline carbonates, silicates, phosphates and'. borates and/or such compounds as the perborate s, persulfates and percarbonates; also organic builders, and. perfumes, coloring matter, preservatives, and
other Substances, mem er. mm deter ent.
compositions.
X ray diffraction patterns showthat the Forms I and II (see Figures 2 ancl 3) represent two dif ferent phases of sodium triphosphate having distin'ctly different crystalline patterns. Those spacings which are particularly useful for the identification of these forms in the presence of other phosphates are indicated on thepatterns,
(8. g; 258,358, 3.71 and 8.1 angstro'n r units in Figure 3 2 (NaSP30m-II) )I Bot forms take. on water to Iorm one and the same hydrate (NaaPaoio' 6H2Q) however, the heat of solution of Form II is much lower than that of Form I, while the Pimmediate solubi1ity"of 'FormII in water is greater than that of Form I. immediate solubility is meant the amount of sodiumtriphosphate in solution at the end of 10 minutes solution time, (i. erthesolu bity determined by inixinginto 100,;milliliters of water. more than the amount of sodiumtriphosphaterequire'dtoniake a saturated solution and cooling to"25''. (3., and at the end of 10 minutes filtering, and evaporating at 105 C. a weighed portion of filtrate followed by drying at 500- C. The weight of dried material obtained per 100 gm. of solution is called the immediate solubilityf). Although various samples of Form II will show identical X-ray diffraction patterns they are frequently observed to differwidely their im;
Table I v Form I II II Variety Rapidhy- Moderate hy- Slow hydrator. drator. drator. Immediate sulubility in 20 30.
gm. per gm. Water soln. 25 0. Hours for hydration in 1% 5,
aqueous detergent mixure.
This table shows two typical examples of the numerous variations encountered in the time,
needed for hydration of Form II sodium triphosphate. These hydration periods were determined by measuring the time'required to reachsubstan tially maximum mass viscosity of the detergentmixture containing the triphosphate as said.
phosphate absorbed the free Water in the mixture:
and converted to the hexahydrate. These measurements were made with a commercially avail-1;
able instrument called the Brabender Plastoe. graph, which records continuously the torsion moment required to rotate a. pair of agitators ins the viscous mixture being examined.
I have found that the hydration of the. tri-.
phosphate in the aqueous detergent mixtures. can readily be accomplished by aging, within the tem-.-. perature range of to 200 F., in a manner. adapted to prevent settling and separation of the undissolved salts.
merous other devices, e. g. screw conveyors. or long pipelines, wherein sufficient storage timeis to be had to permit substantially complete hygdration to the hexahydrate.
Sodium triphosphateis a metastable materialin water solution. It hydrolyzes or reverts,slow-. 1y to form normal and acid salts of other, phOSf.
phoric acids, usually having a higher degree of molecular hydration. Thus: excessively. high temperatures or long aging periods, are to be. avoided since the larger amounts of reversion,
products obtained thereby reduce; the. efficiencyand other desirable properties of q the. final do; tergent composition. In the practice of: this in:- vention it is my purpose to so regulate the op:
erating conditions that reversion of thetriphosphate will be less than 10 percent. The curye in Figure 1 shows conditions of time-and tern peraturefor the aging opfi iation at which;ap; proximatelylo per cent reversion is to;be;,ex;- pected.
The invention will be. better understoodiiro n the following examplesin which allcompositiops are given in terms of percentage by Weight-or;
parts by weight.
Example I .-38 parts of a slowly hydrating; 7
Form II sodium triphosphate, having a part1 size such that it would pass through a, Tyle x with 58 parts of an aqueous fluid containing;
standard 35 mesh screen, were thoroughly; mix
The aging may be eflect-... ed in a vessel equipped With agitators or in nuwater and 24% of sodium alkyl sulfate prepared by sulfating the fatty alcohols obtained by the reduction of coconut oil, and 4 parts of soda ash were then added. The somewhat thin slurry obtained therefrom was mixed thoroughly for 20 minutes and then aged for 6 hours at 165 F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed without incorporating large amounts of air. During the aging the slurry became a viscous but yet pumpable mixture which was then spray dried, in well known manner, yielding a highly satisfactory, rapidly dissolving, efiicient detergent composition in solid granular form, that was free flowing, comparatively dustless, non-sticky and composed of tough granules that did not break down to any significant amount during subsequent packaging operations. Analysis showed it to contain 9% moisture.
The marked benefit obtained through the aging process is shown by comparing the product in Example I with a product obtained by spray drying a like, aqueous, detergent-triphosphate mixture that had not been aged. The latter was a sticky, fragile and dusty product, the particles of which caked and lumped, and broke down badly to form more dust during the packaging operation. This product contained only 3% moisture. Another portion of the same unaged slurry that was spray dried so as to leave 9% moisture in the product gave a damp material that balled badly when handled.
Example II.--32 parts of a moderately slowly hydrating Form II sodium triphosphate, having a particle size such that it would pass through a Tyler standard 35 mesh screen, were thoroughly mixed with 48 parts of an aqueous fluid containing 60% water and 23% sodium alkyl sulfate, and 14 parts of an aqueous fluid containing 65% water and 16.4% of alkyl benzene sulfonate, to which were added 5 parts of soda ash. The somewhat thin slurry obtained therefrom was aged by slowly agitating it for a total of 4 hours at a temperature of 170 F., during which period it gradually became a viscous but yet pumpable mixture. Said slurry was then spray dried in well known manner yielding a highly satisfactory, rapidly dissolving, efficient detergent composition, in solid granular form, that was free flowing, comparatively dustless, non-sticky and comprised of tough granules that did not break down to any significant amount during subsequent packaging operations. Analysis showed it to contain moisture.
A product obtained by spray drying a slurry of like composition, but not aged, was a sticky, fragile and dusty product, the particles of which caked and lumped badly during the packaging operation. This product contained only 4% moisture.
Example III.--36 parts of a poorly hydrating Form II sodium triphosphate were thoroughly mixed with 59 parts of an aqueous fluid containing 60% water and 24% of sodium alkyl sulfate, and 5 parts of soda ash were then added. The somewhat thin slurry obtained therefrom was mixed thoroughly and then aged for 5 hours at 160 F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed without incorporating large amounts of air. During the aging the slurry gradually became a viscous but yet pumpable mixture which was then dried as a film or thin sheet over steam heated rolls,
efficient detergent composition, in diminutive flake form, that was free flowing, non-sticky and comprised of tough particles that did not break down to any significant amount durin subsequent handling. Analysis showed the product contained 14% moisture.
Example IV..29 parts of a slowly hydrating Form II sodium triphosphate, having a particle size such that it would pass through a Tyler standard 35 mesh screen, were thoroughly mixed with 68 parts of an aqueous fluid containing 65% water and 16.3% of alkyl benzene sulfonate, to which were added 5 parts of soda ash. The somewhat thin slurry obtained therefrom was mixed thoroughly for 20 minutes and then aged for 6 hours at F. during which time it was agitated by a slowly turning (15 R. P. M.) paddle type agitator that served to keep the slurry well mixed. The mixture, which became more viscous during aging, was then spray dried in well known manner, yielding a highly satisfactory, rapidly dissolving, effiicient detergent composition in solid granular form, that was free flowing, comparatively dustless, non-sticky and comprised of tough granules that did not break down to any significant amount during subsequent packaging operations. Analysis showed it to contain 7% moisture.
A product obtained by spray drying a slurry of like composition, but not aged, was a sticky,
fragile and dusty product, the particles of which lumped very badly during the packaging operation. This product contained only 3% moisture.
It will be noted that in the detergent composition of each of the foregoing examples the Form II triphosphate is a major component and was, in fact, present in greater quantity than the organic detergent.
I have found that an aging period of six hours at 165 C. is, in most cases, sufiicient for the treatment of commercial phase II sodium triphosphate used in the preparation of detergent compositions as hereinbefore described, and that with occasional lots, which represent moderately fast hydrating varieties, as little as one to two hours treatment will sufiice; however, since an intent of the aging is to substantially complete the hydration of the triphosphate to the hexahydrate I generally employ such periods of time as are necessary to completely hydrate extremely slowly hydrating varieties of Form II that are infrequently encountered.
In the preceding specific examples detergents of each of the various types enumerated in de-- fining the term may be substituted for the deproportion of triphosphate is used, very little of the triphosphate is in solution at any one time during the processing operations, most of t being merely suspended as a slurry. Thus to insure the desired product solubility rate the triphosphate used should in general have a particle size no larger than that desired in the final product.
This invention in its broad aspects is not restricted to the manufacture of detergent mixture'si containing in,..addition.- tootheorganicr dee. tergentonly; sodium triphosphatee but .mayalso be. applied ;in the manufacture .of 1 detergents comprising triphosphates .of potassiumand' other. alkali: metals.
tion in; which thealkali metal triphosphatemay be; included, suclr as. flakes. threads, powdersi or.
spraydriedlforma It-js to, be .understood that .the .foregoing. more.
articularly described.processes; are to, be. con..-. sidered as, illustrative of .the preferred .method only; such changes. and modifications therein. are contemplated; as,v would; normally occurv to those; skilled in therart, to. which. the invention 4 relates,
Having thus describedmyinvention, what. I claim; and desire to secure byv LettersPatentis: 1. Inthe process. of; manufacturing: a. heat dried detergent. composition. substantially. free ofdust; and: of stickiness, and. caking properties,
the steps of incorporating: Form. II1sodium..tri.-. phosphate ina fluid mixture. containing. essen-.
tially -an; organic; detergent. ofzthe. group consist-- ing of;. alkali. metal soaps and: Water soluble nonsoapwsynthetic detergents. and more than. sufficient: w'aterto effect substantially complete-11y" dration of the said triphosphate-to the hexahydrate, the amount, of, said "triph osphate incor: porated beinginexcessof the. amount of detergent; agitating and. aging the. mixture withinthe temperature range'of 120 to 200 F. for-at least one. hour. and until hydration to-the hexahydrate is substantiallycompleteas determine} bleby measuring the time required to reach a maximumin a mass -.viscosity test of a likemi g ture. of. said components, but no longer than thattimerepresented by the pointon the curve.
in Figure 1 which corresponds to 10 percent reversion of= the triphosphate at the aging tem perature employed; and heat drying the aged mixtureto the'solid form."
2: n th r qce e o manufacturing a heatdried detergent me e i n .s h ant l y reeof du t and of stickinessand caking properties the steps of incorporating Form 'I'I 'so'diunr triphosphate in a fluid detergent mixture containingnasf the .w te rsqlub ..salt of amember selected from theglfgl ll. consisting .50 ,.mi .tu'r s thereci containingfrom s to'18ca 0 atszms intheallgyl active detergent ingredient of Sulfuric t ie Pre i cts. o a k l. and s b stituted- 'allg'yl *cornpounds,
roup, and morethan su tertoefie'ct ls fi i llrz mele e.hrdretien e idi phosp at g h hexah-x rate..theamemt e Nor f is. it, limited to. any par. ticular type of manufactured .detergentcomposie;
.. 5 I iaiif ih eee ei hqern rated.bein .i e ceseoi the amount of:detergent;- agitating and aging the mixture within the temperature rangeiof 120 to 200?:F.afor at.least oneihour and until hydration to the hexahydrateis substantially complete as determinable by measuring the time required to reach -amaximum in a mass'viscosity test of a likemixture of said-components, but no longer than-that time representedby the point on the curvein Figure- 1 which corresponds to 10 percent reversion of the triphosphate'at' the aging" temperature employed; and heat dry-ing'the aged mixture tothe solid form-.
3. In the process of manufacturinga heat dried detergent composition substantially free of dust and-of-stiokiness and caking-properties; the steps of incorporating Form II-sodiumtriphosphate in a fluidmixture containing essentially an organic detergentof the group consisting of alkali-metal soaps and water soluble-non-soap" syntheticde tergents and more than sufiicient water to efiegt substantiallycompletehydration of the said triphosphate; the amount-of said triphosphate incorporated being in excess of: the amount of detergent; agitating and aging the mixture withp in the temperature range of l29 200? F; for at,
least one hour and until hydration is substantially complete as determinable by measuring the time required to reach a maximum in a mass. viscositytestof a like mixture of saidcomponents, but no longer than that time represented by the point onthe curvein Figure 1 which corresponds to the aging temperature employed; and heatdrying the aged mixture to the solid form.
EDBEBT HIZER REFERENCES: CITED' The follow-ing references ;;are of-reoord in the file of this patent:
Claims (1)
1. IN THE PROCESS OF MANUFACTURING A HEAT DRIED DETERGENT COMPOSITION SUBSTANTIALLY FREE OF DUST AND OF STICKNESS AND CAKING PRPERTIES, THE STEPS OF INCORPORATING FORM 22 SODIUM TRIPHOSPHATE IN A FLUID MIXTURE CONTAINING ESSENTIALLY AN ORGANIC DETERGENT OF THE GROUP CONSISTING OF ALKALI METAL SOAPS AND WATER SOLUBLE NONSOAP SYNTHETIC DETERGENTS AND MORE THAN SUFFICIENT WATER TO EFFECT SUBSTANTIALLY COMPLETE HYDRATION OF THE SAID TRIPHOSPHATE TO THE HEXAHYDRATE, THE AMOUNT OF SAID TRIPHOSPHATE INCORPORATED BEING IN EXCESS OF THE AMOUNT OF DETERGENT; AGITATING AND AGING THE MIXTURE WITHIN THE TEMPERATURE RANGE OF 120* TO 200* F. FOR AT LEAST ONE HOUR AND UNTIL HYDRATION TO THE HEXAHYDTRATE IS SUBSTANTIALLY COMPLETE AS DETERMINABLE BY MEASURING THE TIME REQUIRED TO REACH A MAXIMUM IN A MASS VISCOSITY TEST OF A LIKE MIXTURE OF SAID COMPONENTS, BUT NO LONGER THAN THAT TIME REPRESENTED BY THE POINT ON THE CURVE IN FIGURE 1 WHICH CORRESPONDS TO 10 PER CENT REVERSION OF THE TRIPHOSHPATE AT THE AGING TEMPERATURE EMPLOYED; AND HEAT DRYING THE AGED MIXTURE TO THE SOLID FORM.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US31174A US2622068A (en) | 1948-06-04 | 1948-06-04 | Process of making heat dried detergent compositions containing form ii sodium triphosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US31174A US2622068A (en) | 1948-06-04 | 1948-06-04 | Process of making heat dried detergent compositions containing form ii sodium triphosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2622068A true US2622068A (en) | 1952-12-16 |
Family
ID=21858011
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US31174A Expired - Lifetime US2622068A (en) | 1948-06-04 | 1948-06-04 | Process of making heat dried detergent compositions containing form ii sodium triphosphate |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2622068A (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2861954A (en) * | 1956-01-09 | 1958-11-25 | Lever Brothers Ltd | Polyphosphate compositions containing soap and 2-mercaptothiazoline |
| US2864770A (en) * | 1956-10-03 | 1958-12-16 | Procter & Gamble | Liquid detergent composition |
| US2874123A (en) * | 1954-09-07 | 1959-02-17 | Colgate Palmolive Co | Process for the preparation of granular compositions |
| US2897155A (en) * | 1955-07-27 | 1959-07-28 | Lever Brothers Ltd | Process for preparing a detergent composition containing anhydrous form 11 tripolyphosphate |
| US2904513A (en) * | 1954-04-16 | 1959-09-15 | Monsanto Chemicals | Inorganic phosphate compositions, and methods for the preparation and utilization thereof |
| US2959554A (en) * | 1956-04-11 | 1960-11-08 | Olin Mathieson | Bleaching composition |
| US2961409A (en) * | 1957-04-02 | 1960-11-22 | Procter & Gamble | Process for preparing detergent compositions |
| US2961410A (en) * | 1957-04-02 | 1960-11-22 | Procter & Gamble | Process for preparing detergent compositions |
| US2977317A (en) * | 1954-10-21 | 1961-03-28 | Knapsack Ag | Process for producing compositions containing sodium tripolyphosphate |
| US3056652A (en) * | 1957-11-26 | 1962-10-02 | Lever Brothers Ltd | Modification of the hydration characteristics of form ii sodium tripolyphosphate prior to detegent processing |
| US3133024A (en) * | 1961-03-14 | 1964-05-12 | Monsanto Chemicals | Heat-dried detergent processes |
| US3272752A (en) * | 1961-03-07 | 1966-09-13 | Knapsack Ag | Method of producing detergents |
| US3303134A (en) * | 1961-09-05 | 1967-02-07 | Monsanto Co | Detergent processes and compositions therefor |
| US3338671A (en) * | 1963-06-20 | 1967-08-29 | Fmc Corp | Sodium tripolyphosphate granular product |
| US3390093A (en) * | 1962-06-06 | 1968-06-25 | Monsanto Co | Detergent compositions containing hydrated alkali metal tripolyphosphates |
| US3423321A (en) * | 1964-07-17 | 1969-01-21 | Monsanto Co | Detergent processes |
| US3461074A (en) * | 1965-10-22 | 1969-08-12 | United States Borax Chem | Detergent compositions |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US912622A (en) * | 1909-02-16 | William E Ridenour | Manufacture of hydrated sodium carbonate. | |
| US1046847A (en) * | 1912-03-09 | 1912-12-10 | William Reginald Ormandy | Process of manufacturing detergents. |
| GB490285A (en) * | 1937-01-11 | 1938-08-11 | Ig Farbenindustrie Ag | Manufacture of washing agents |
| US2206289A (en) * | 1936-07-02 | 1940-07-02 | Diamond Alkali Co | Stable, hydrous, alkaline silicates |
| US2365215A (en) * | 1944-12-19 | Detergent composition | ||
| US2365190A (en) * | 1944-12-19 | Washing compositions | ||
| US2374100A (en) * | 1937-05-03 | 1945-04-17 | Hall Lab Inc | Water treatment |
| US2396918A (en) * | 1938-11-04 | 1946-03-19 | Monsanto Chemicals | Water-treating composition |
| US2423451A (en) * | 1943-09-28 | 1947-07-08 | Colgate Palmolive Peet Co | Soap product and method of making same |
| US2427642A (en) * | 1942-05-28 | 1947-09-16 | Westvaco Chlorine Products Cor | Rapidly soluble tetrasodium pyrophosphate |
| US2480730A (en) * | 1949-08-30 | Method of producing a free-flowing |
-
1948
- 1948-06-04 US US31174A patent/US2622068A/en not_active Expired - Lifetime
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US912622A (en) * | 1909-02-16 | William E Ridenour | Manufacture of hydrated sodium carbonate. | |
| US2365215A (en) * | 1944-12-19 | Detergent composition | ||
| US2365190A (en) * | 1944-12-19 | Washing compositions | ||
| US2480730A (en) * | 1949-08-30 | Method of producing a free-flowing | ||
| US1046847A (en) * | 1912-03-09 | 1912-12-10 | William Reginald Ormandy | Process of manufacturing detergents. |
| US2206289A (en) * | 1936-07-02 | 1940-07-02 | Diamond Alkali Co | Stable, hydrous, alkaline silicates |
| GB490285A (en) * | 1937-01-11 | 1938-08-11 | Ig Farbenindustrie Ag | Manufacture of washing agents |
| US2374100A (en) * | 1937-05-03 | 1945-04-17 | Hall Lab Inc | Water treatment |
| US2396918A (en) * | 1938-11-04 | 1946-03-19 | Monsanto Chemicals | Water-treating composition |
| US2427642A (en) * | 1942-05-28 | 1947-09-16 | Westvaco Chlorine Products Cor | Rapidly soluble tetrasodium pyrophosphate |
| US2423451A (en) * | 1943-09-28 | 1947-07-08 | Colgate Palmolive Peet Co | Soap product and method of making same |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2904513A (en) * | 1954-04-16 | 1959-09-15 | Monsanto Chemicals | Inorganic phosphate compositions, and methods for the preparation and utilization thereof |
| US2874123A (en) * | 1954-09-07 | 1959-02-17 | Colgate Palmolive Co | Process for the preparation of granular compositions |
| US2977317A (en) * | 1954-10-21 | 1961-03-28 | Knapsack Ag | Process for producing compositions containing sodium tripolyphosphate |
| US2897155A (en) * | 1955-07-27 | 1959-07-28 | Lever Brothers Ltd | Process for preparing a detergent composition containing anhydrous form 11 tripolyphosphate |
| US2861954A (en) * | 1956-01-09 | 1958-11-25 | Lever Brothers Ltd | Polyphosphate compositions containing soap and 2-mercaptothiazoline |
| US2959554A (en) * | 1956-04-11 | 1960-11-08 | Olin Mathieson | Bleaching composition |
| US2864770A (en) * | 1956-10-03 | 1958-12-16 | Procter & Gamble | Liquid detergent composition |
| US2961409A (en) * | 1957-04-02 | 1960-11-22 | Procter & Gamble | Process for preparing detergent compositions |
| US2961410A (en) * | 1957-04-02 | 1960-11-22 | Procter & Gamble | Process for preparing detergent compositions |
| US3056652A (en) * | 1957-11-26 | 1962-10-02 | Lever Brothers Ltd | Modification of the hydration characteristics of form ii sodium tripolyphosphate prior to detegent processing |
| US3272752A (en) * | 1961-03-07 | 1966-09-13 | Knapsack Ag | Method of producing detergents |
| US3133024A (en) * | 1961-03-14 | 1964-05-12 | Monsanto Chemicals | Heat-dried detergent processes |
| US3303134A (en) * | 1961-09-05 | 1967-02-07 | Monsanto Co | Detergent processes and compositions therefor |
| US3390093A (en) * | 1962-06-06 | 1968-06-25 | Monsanto Co | Detergent compositions containing hydrated alkali metal tripolyphosphates |
| US3338671A (en) * | 1963-06-20 | 1967-08-29 | Fmc Corp | Sodium tripolyphosphate granular product |
| US3423321A (en) * | 1964-07-17 | 1969-01-21 | Monsanto Co | Detergent processes |
| US3461074A (en) * | 1965-10-22 | 1969-08-12 | United States Borax Chem | Detergent compositions |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US2622068A (en) | Process of making heat dried detergent compositions containing form ii sodium triphosphate | |
| US3912649A (en) | Detergent composition employing alkali metal polysilicates | |
| US4025609A (en) | Process for preparing stable sodium percarbonate | |
| US3971631A (en) | Pelletizing alkali metal polysilicates | |
| US3971727A (en) | Alkali metal polysilicates, methods for their production and detergent compositions employing same | |
| WO1990004629A2 (en) | Process for manufacturing tenside-containing granulates | |
| US2712529A (en) | Detergent composition | |
| US3441374A (en) | Alkali metal condensed phosphate materials,processes for preparing same and resulting compositions | |
| US2864770A (en) | Liquid detergent composition | |
| US2717243A (en) | Non-caking alkyl aryl sulfonate | |
| US3247118A (en) | Method for preparing detergent compositions | |
| US2940938A (en) | Process of making a colloidal suspension of phosphates | |
| DE2529685B2 (en) | METHOD FOR PRODUCING LOW PHOSPHATE OR PHOSPHATE-FREE DETERGENT OR CLEANING AGENTS | |
| US3054656A (en) | Process for the production of improved sodium tripolyphosphate | |
| US2961410A (en) | Process for preparing detergent compositions | |
| US2351559A (en) | Process for the preparation of | |
| US2647064A (en) | Method of improving the cold-water solubility of a fibrous cellulose ether | |
| US2776943A (en) | Treatment of soap particles | |
| US2298651A (en) | Particulate solid detergent | |
| US3174934A (en) | Hydration of sodium tripolyphosphate | |
| US3849346A (en) | Process for preparing granular detergent composition | |
| US2746930A (en) | Process for making detergent compositions | |
| US2961409A (en) | Process for preparing detergent compositions | |
| US2480730A (en) | Method of producing a free-flowing | |
| US5306478A (en) | Preparation of granular compositions |