US2895916A - Method for preparing detergent compositions - Google Patents

Method for preparing detergent compositions Download PDF

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Publication number
US2895916A
US2895916A US585017A US58501756A US2895916A US 2895916 A US2895916 A US 2895916A US 585017 A US585017 A US 585017A US 58501756 A US58501756 A US 58501756A US 2895916 A US2895916 A US 2895916A
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United States
Prior art keywords
phosphate
mixture
water
silicate
detergent
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
Application number
US585017A
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English (en)
Inventor
Joseph A Milenkevich
James E Henjum
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.)
Procter and Gamble Co
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Procter and Gamble Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to NL217279D priority Critical patent/NL217279A/xx
Priority to DENDAT1050005D priority patent/DE1050005B/de
Priority to BE557388D priority patent/BE557388A/xx
Priority to US585017A priority patent/US2895916A/en
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Priority to AT302757A priority patent/AT210543B/de
Priority to ES0235418A priority patent/ES235418A1/es
Priority to GB15186/57A priority patent/GB809102A/en
Priority to CH4613057A priority patent/CH368568A/fr
Priority to FR1175203D priority patent/FR1175203A/fr
Application granted granted Critical
Publication of US2895916A publication Critical patent/US2895916A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/395—Bleaching agents
    • C11D3/3958—Bleaching agents combined with phosphates

Definitions

  • This invention relates toA a method for preparing deter-gent compositions.
  • this invention relates to a method for preparing detergent compositions which are particularly useful in automatic dishwashing machines.
  • compositions comprising in combination an alkaline detergent salt (eg. sodium metasilicate), an alkaline condensed phosphate (e.g. sodium tripolyphosphate), and chlorinated trisodium phosphate have been suggested as having particular utility for dishwashing applications (U.S. Letters Patent 2,689,225).
  • alkaline detergent salt eg. sodium metasilicate
  • alkaline condensed phosphate e.g. sodium tripolyphosphate
  • chlorinated trisodium phosphate e.g. sodium phosphate
  • the formulation of such compositions which are made up of agglomerates of the various ingredients, has heretofore been accomplished through the addition of aqueous silicate to a mechanical mixture of alkaline condensed phosphate and chlorinated trisodium phosphate.
  • alkali metal silicate indicates those silicates having an average Si02/ alkali metal oxide ratio of about 2.0 to 3.4 and includes mixtures of silicates having dissimilar SiO2/ alkali metal ⁇ oxide ratios.
  • chlorinated trisodium phosphate is used to designate a composition consisting of trisodium phosphate and sodium hypochlorite in intimate association in a crystalline form.
  • the chlorinated trisodium phosphate may contain from 1% to 5% available chlorine and may be prepared by the methods of U.S. Letters Patent 1,555,474 or 1,965,- 304, or modifications thereof.
  • rPhe essence of our invention lies in the particular rsequence in which the various constituents of the detergent compositions are admixed.
  • the particular sequence of steps herein described must be closely adhered to.
  • a dishwashing composition comprising, by weight, 45 parts sodium tripolyphosphate, 32 parts of a 41% aqueous solution of sodium silicate having an average SiO2/Na20 ratio of about 2.9, and 20 parts chlorinated trisodium phosphate was prepared in accordance with the process of our invention in the following manner:
  • the sodium tripolyphosphate in a substantially anhydrous condition, and at room temperature, was placed Iin a ribbon mixer wherein the sodium silicate in the form of a 41% aqueous solution, heated to a temperature of about 1GO-120 F. to control viscosity, was sprayed onto the phosphate while it was being agitated.
  • the addition of the aqueous silicate caused hydration of the ⁇ tripolyphosphate to ⁇ take place with the evolution of heat. Consequently, in ⁇ order to maintain the phosphate-silicate mixture in a non-liquid condition, precautions were taken to prevent the temperature of the mix from rising above about F.
  • silicates can be used, the average SiO2/ alkali metal oxide ratio of such silicates as we have found suitable being in the range from about 2.0 to about 3.4 and more preferably in the range from about 2.7 to about 2.9.V y I These silicates can be added inlour process in a number of diiferentways.
  • a non-ionic detergent such as the Pluronics -(condensates.of.ethy1ene oxidewith afhydrophobic base i of a non-ionic detergent agent( Also, we have found that some additional benefits Yin formed by condensing propylene oxide with propylene glycol-marketed by Wyandotte Chemicals Corp.) or the Hyonics (e.g. fatty alkylolamides-'marketed by Nopco Chemical Co.) can be used in conjunction with the aforementioned constituents in a detergent composition.
  • Detergent compositions which can be advantageously prepared our process comprise in combination from about% to about 60% alkaline condensed phosphate, from about 8% to about 20% alkali metal silicate as silicate solids, and from about 15% Vto about 30% of chlorinated trisodium phosphate with or without the addition product caking and gumming .orA gelling characteristics can'be'obtained by adding other ingredients to the deter,-V
  • salts as urea and potassium nitrate, hyi drated salts such'as hydrated ortho, pyro, and tripolyphosphate, and inertdiluents such assilica andtalc.
  • Example I f poured, atroom temperature, over the phosphates, while they were being agitated, during aperiod of about 3 minutes.”
  • silicate addition agglomerates ranging Vfrom the size ofY grains of sand to marbles formed, while the temperature of the mixture rose from 82 to 95 F.
  • n n A second detergent composition was prepared in ac- Vcordance' with the above procedure except that the sil- Yicate solution was Yadded'prior to theaddition of the chlorinated trisodium phosphate. During the silicate addition, the temperature in the mixer rose from 84 to 114" ⁇ F. and then dropped to 108 F. after a 15-minute aging period. 'Ihe pouring characteristics of the product were observed in the Ysame manner as above described.
  • detergent compositions comprising an Valkaline condensed phosphate, anY alkali-metal silicate, and chlorinated trisodium phosphate, when prepared by adding aqueous silicate ⁇ to a mechanical mixture ofthe the phosphates, tend to -form a gum or gel in use and that Vthis characteristic is particularly evident when'such composition is used in a dishwashing machine having two -wash cycles.
  • V vIn the followingexamples a comparison is made of the gumming and/ or gelling tendencies of detergent compositions prepared by the above method and by the method of our invention. Since this characteristic can ybe appropriately evaluated through practical use in an automatic dishwasher utilizing twowarsh cycles, the data appearing in the subsequent examples were obtained through this medium.
  • the particular dishwashing machine used for the evaluations had two separate detergent cups, each having aV capacity of. about 20 cc., which were filled with the productto be tested.
  • the machine cycle was as follows: First wash, second wash; first rinse; second rinse.
  • the detergent in one of the cups was washed out by the water action in the machine and was utilized in this Wash cycle.
  • the detergent in the second cup was protected against Washing out but did come into contact with steam and sprayA during the first wash cycle.
  • ⁇ the detergent in the second cup was made available to the water action in the machine and was washed out of the cup and utilized in this second Wash.
  • Thedegree of gumming and/ or gelling was determined by observing the proportionate amount of detergent retained by lthe second cup after each of the second wash, rst rinse, and second rinse cycles.
  • Example 2 The detergent compositions prepared in accordance with -the processes outlined in Example 1 after aging for two hours were used in a dishwasher of the type described above;
  • the figuresk appearing in the table below Krepresent the proportionate amount of detergent retained in the second detergent cup after completion of It may be readily seen from the above data that the process of our invention results in a detergent product which has remarkably superior resistance to gumming or gelling.
  • Example 3 A number of detergent compositions, each comprising 45 parts by weight sodium tripolyphosphate, 32 parts by weight of a 41% aqueous solution of sodium silicate having an average SiO2/Na20 ratio of 2.9, and 20 parts by weight of chlorinated trisodium phosphate, were prepared according to the following general processes. In all cases, subsequent to the addition of the last product constituent, the products were aged for about 15 minutes during which time they were intermittently agitated, and the resultant agglomerates were reduced in size to pass a -mesh Tyler screen.
  • Sample A The sodium silicate, in the form of a 41% aqueous solution, was added to a mechanical mixture of the sodium tripolyphosphate and chlorinated trisodium phosphate.
  • Sample B The sodium silicate, in the form of a 41% aqueous solution, was added to the sodium tripolyphosphate prior to the addition thereto of the chlorinated trisodium phosphate.
  • Sample C.-90% of the total aqueous sodium silicate solution to be used was added to the tripolyphosphate prior to the addition thereto of the chlorinated trisodium phosphate. The remaining 10% of the silicate solution was added subsequent to the chlorinated trisodium phosphate addition.
  • Sample D.-70% of the total aqueous sodium silicate solution was added prior to the chlorinated trisodium phosphate addition and the remaining 30% was added subsequent to the chlorinated trisodium phosphate addition.
  • a process VforY preparing detergent jcompositions comprising a Waterfsoluble alkaline condensed phosphate, ,a Water-soluble alkali Ynietal silicate, and chlorinated trisodium phosphate which comprises adding to a substantially anhydrous alkaline condensed phosphate an aqueous solution Vof an alkali metal silicatehaving an average SiOz/alkali metalv oxide ratio inthe range from about 2.0 to about 3.4, the amount of said'silicate solution lcomprising at least 50%N of the total amount of silicate solution to'be added, the vtotal amount of moisture in said aqueous silicate solution being at least adequate to wet the fsaid condensed phosphate suiciently.

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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)
US585017A 1956-05-15 1956-05-15 Method for preparing detergent compositions Expired - Lifetime US2895916A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
NL217279D NL217279A (ja) 1956-05-15
DENDAT1050005D DE1050005B (ja) 1956-05-15
BE557388D BE557388A (ja) 1956-05-15
US585017A US2895916A (en) 1956-05-15 1956-05-15 Method for preparing detergent compositions
AT302757A AT210543B (de) 1956-05-15 1957-05-08 Verfahren zur Herstellung von Reinigungsmittelgemischen
ES0235418A ES235418A1 (es) 1956-05-15 1957-05-11 Procedimiento para la preparacion de composiciones detergentes
GB15186/57A GB809102A (en) 1956-05-15 1957-05-13 Preparation of detergent compositions
CH4613057A CH368568A (fr) 1956-05-15 1957-05-15 Procédé de préparation d'une composition détergente
FR1175203D FR1175203A (fr) 1956-05-15 1957-05-15 Procédé pour la préparation de compositions détersives

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US585017A US2895916A (en) 1956-05-15 1956-05-15 Method for preparing detergent compositions

Publications (1)

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US2895916A true US2895916A (en) 1959-07-21

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US585017A Expired - Lifetime US2895916A (en) 1956-05-15 1956-05-15 Method for preparing detergent compositions

Country Status (9)

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US (1) US2895916A (ja)
AT (1) AT210543B (ja)
BE (1) BE557388A (ja)
CH (1) CH368568A (ja)
DE (1) DE1050005B (ja)
ES (1) ES235418A1 (ja)
FR (1) FR1175203A (ja)
GB (1) GB809102A (ja)
NL (1) NL217279A (ja)

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2979464A (en) * 1956-11-09 1961-04-11 Degussa Perborate granulation
US3054656A (en) * 1958-12-04 1962-09-18 Fmc Corp Process for the production of improved sodium tripolyphosphate
US3058917A (en) * 1959-07-28 1962-10-16 Hagan Chemicals & Controls Inc Liquid dishwashing detergent
US3110677A (en) * 1959-04-23 1963-11-12 Olin Mathieson Chlorinated trisodium phosphate
US3166512A (en) * 1961-04-06 1965-01-19 Economics Lab Stable, solid chlorinated caustic product containing available chlorine and method of preparation thereof
US3247118A (en) * 1963-02-25 1966-04-19 Lever Brothers Ltd Method for preparing detergent compositions
US3248330A (en) * 1963-05-24 1966-04-26 Monsanto Co Process for preparing a stable, freeflowing dishwashing composition
US3306858A (en) * 1965-06-17 1967-02-28 Economics Lab Process for the preparation of storage stable detergent composition
US3314891A (en) * 1964-05-27 1967-04-18 Wyandotte Chemicals Corp Low foaming detergent
US3359207A (en) * 1965-06-18 1967-12-19 Wyandotte Chemicals Corp Chlorine-stable detergent compositions and process for the preparation thereof
US3361675A (en) * 1965-08-23 1968-01-02 Fmc Corp Dry-mixed detergent compositions
US3520815A (en) * 1969-09-04 1970-07-21 Grace W R & Co Process of preparing stable detergent composition
US4169806A (en) * 1978-08-09 1979-10-02 The Procter & Gamble Company Agglomeration process for making granular detergents
US4207197A (en) * 1978-08-09 1980-06-10 The Procter & Gamble Company Agglomeration process for making granular detergents
US4228025A (en) * 1979-06-29 1980-10-14 The Procter & Gamble Company Agglomeration process for making granular detergents
US4421664A (en) * 1982-06-18 1983-12-20 Economics Laboratory, Inc. Compatible enzyme and oxidant bleaches containing cleaning composition
US4427417A (en) 1982-01-20 1984-01-24 The Korex Company Process for preparing detergent compositions containing hydrated inorganic salts
US4601844A (en) * 1984-08-31 1986-07-22 The Procter & Gamble Company Granular automatic dishwasher detergent with alkyl phosphate and calcium ion source
US4832862A (en) * 1986-05-27 1989-05-23 Rhone-Poulenc Chimie Composite detergent particulates
US4844831A (en) * 1987-03-30 1989-07-04 Rhone-Poulenc Chimie Use of metasilicate/silica combination granulate in detergent compositions for washing machines
US5612305A (en) * 1995-01-12 1997-03-18 Huntsman Petrochemical Corporation Mixed surfactant systems for low foam applications
US5614485A (en) * 1990-07-10 1997-03-25 The Procter & Gamble Company Process for making a granular dishwashing composition by agglomerating ingredients and admixing solid alkali metal silicate
US5616277A (en) * 1991-08-13 1997-04-01 The Procter & Gamble Company Incorporating nonionic surfactant into silicate for granular automatic dishwashing detergent composition
US5914307A (en) * 1996-10-15 1999-06-22 The Procter & Gamble Company Process for making a high density detergent composition via post drying mixing/densification
EP2520641A1 (en) 2005-06-30 2012-11-07 The Procter & Gamble Company Low phosphate automatic dishwashing detergent composition

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH471891A (de) * 1963-12-31 1969-04-30 Unilever Nv Verfahren zur Herstellung einer Reinigungsmitteltablette
SE424739B (sv) * 1977-05-26 1982-08-09 Elektrokemiska Ab Granuler ravara for maskindiskmedel-, avfettningsmedel-, och rengorings-medelskomposition och forfarande for dess framstellning

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1988991A (en) * 1932-02-19 1935-01-22 Firm Henkel & Cie Gmbh Manufacture of solid products containing alkali hypochlorite
US2034361A (en) * 1929-03-23 1936-03-17 Roy C Sutton Alkaline detergent powder and method of making the same
US2324302A (en) * 1940-05-31 1943-07-13 Diversey Corp Stable-colored crystalline alkali metal hypochlorite-containing composition
US2333444A (en) * 1943-11-02 Method op preparing stable deter
US2473822A (en) * 1949-06-21 Method of making same
US2524394A (en) * 1946-12-23 1950-10-03 Samuel L Madorsky Method of manufacturing stable alkali hypochlorite compositions
US2689225A (en) * 1954-09-14 Detergent compositions
US2712529A (en) * 1948-10-21 1955-07-05 Procter & Gamble Detergent composition

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2333444A (en) * 1943-11-02 Method op preparing stable deter
US2473822A (en) * 1949-06-21 Method of making same
US2689225A (en) * 1954-09-14 Detergent compositions
US2034361A (en) * 1929-03-23 1936-03-17 Roy C Sutton Alkaline detergent powder and method of making the same
US1988991A (en) * 1932-02-19 1935-01-22 Firm Henkel & Cie Gmbh Manufacture of solid products containing alkali hypochlorite
US2324302A (en) * 1940-05-31 1943-07-13 Diversey Corp Stable-colored crystalline alkali metal hypochlorite-containing composition
US2524394A (en) * 1946-12-23 1950-10-03 Samuel L Madorsky Method of manufacturing stable alkali hypochlorite compositions
US2712529A (en) * 1948-10-21 1955-07-05 Procter & Gamble Detergent composition

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2979464A (en) * 1956-11-09 1961-04-11 Degussa Perborate granulation
US3054656A (en) * 1958-12-04 1962-09-18 Fmc Corp Process for the production of improved sodium tripolyphosphate
US3110677A (en) * 1959-04-23 1963-11-12 Olin Mathieson Chlorinated trisodium phosphate
US3058917A (en) * 1959-07-28 1962-10-16 Hagan Chemicals & Controls Inc Liquid dishwashing detergent
US3166512A (en) * 1961-04-06 1965-01-19 Economics Lab Stable, solid chlorinated caustic product containing available chlorine and method of preparation thereof
US3247118A (en) * 1963-02-25 1966-04-19 Lever Brothers Ltd Method for preparing detergent compositions
US3248330A (en) * 1963-05-24 1966-04-26 Monsanto Co Process for preparing a stable, freeflowing dishwashing composition
US3314891A (en) * 1964-05-27 1967-04-18 Wyandotte Chemicals Corp Low foaming detergent
US3306858A (en) * 1965-06-17 1967-02-28 Economics Lab Process for the preparation of storage stable detergent composition
US3359207A (en) * 1965-06-18 1967-12-19 Wyandotte Chemicals Corp Chlorine-stable detergent compositions and process for the preparation thereof
US3361675A (en) * 1965-08-23 1968-01-02 Fmc Corp Dry-mixed detergent compositions
US3520815A (en) * 1969-09-04 1970-07-21 Grace W R & Co Process of preparing stable detergent composition
US4169806A (en) * 1978-08-09 1979-10-02 The Procter & Gamble Company Agglomeration process for making granular detergents
US4207197A (en) * 1978-08-09 1980-06-10 The Procter & Gamble Company Agglomeration process for making granular detergents
US4228025A (en) * 1979-06-29 1980-10-14 The Procter & Gamble Company Agglomeration process for making granular detergents
US4427417A (en) 1982-01-20 1984-01-24 The Korex Company Process for preparing detergent compositions containing hydrated inorganic salts
US4421664A (en) * 1982-06-18 1983-12-20 Economics Laboratory, Inc. Compatible enzyme and oxidant bleaches containing cleaning composition
US4601844A (en) * 1984-08-31 1986-07-22 The Procter & Gamble Company Granular automatic dishwasher detergent with alkyl phosphate and calcium ion source
US4832862A (en) * 1986-05-27 1989-05-23 Rhone-Poulenc Chimie Composite detergent particulates
US4844831A (en) * 1987-03-30 1989-07-04 Rhone-Poulenc Chimie Use of metasilicate/silica combination granulate in detergent compositions for washing machines
US5614485A (en) * 1990-07-10 1997-03-25 The Procter & Gamble Company Process for making a granular dishwashing composition by agglomerating ingredients and admixing solid alkali metal silicate
US5616277A (en) * 1991-08-13 1997-04-01 The Procter & Gamble Company Incorporating nonionic surfactant into silicate for granular automatic dishwashing detergent composition
US5612305A (en) * 1995-01-12 1997-03-18 Huntsman Petrochemical Corporation Mixed surfactant systems for low foam applications
US5914307A (en) * 1996-10-15 1999-06-22 The Procter & Gamble Company Process for making a high density detergent composition via post drying mixing/densification
EP2520641A1 (en) 2005-06-30 2012-11-07 The Procter & Gamble Company Low phosphate automatic dishwashing detergent composition
EP3450533A1 (en) 2005-06-30 2019-03-06 The Procter & Gamble Company Low phosphate automatic dishwashing detergent composition

Also Published As

Publication number Publication date
CH368568A (fr) 1963-04-15
GB809102A (en) 1959-02-18
DE1050005B (ja)
BE557388A (ja)
FR1175203A (fr) 1959-03-23
AT210543B (de) 1960-08-10
ES235418A1 (es) 1957-11-16
NL217279A (ja)

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