US3344076A - Process for preparing detergent tablets - Google Patents

Process for preparing detergent tablets Download PDF

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Publication number
US3344076A
US3344076A US183021A US18302162A US3344076A US 3344076 A US3344076 A US 3344076A US 183021 A US183021 A US 183021A US 18302162 A US18302162 A US 18302162A US 3344076 A US3344076 A US 3344076A
Authority
US
United States
Prior art keywords
tablets
detergent
weight
minutes
mixture
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
US183021A
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English (en)
Inventor
Jr Edward D Wilcox
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.)
Lever Brothers Co
Original Assignee
Lever Brothers 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 CA733929A priority Critical patent/CA733929A/en
Application filed by Lever Brothers Co filed Critical Lever Brothers Co
Priority to US183021A priority patent/US3344076A/en
Priority to FR929480A priority patent/FR1357206A/fr
Priority to BE646800A priority patent/BE646800A/xx
Application granted granted Critical
Publication of US3344076A publication Critical patent/US3344076A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • 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

Definitions

  • the detergent tablets contain two classes of essential components, namely nonionic detergent and phosphate, which are used in certain critical amounts and have a certain critical nature as set forth hereinafter.
  • the detergent briquettes contain from about 4% to about 13% by Weight, and preferably from about to about 12% by weight, of one or more synthetic organic nonionic nonsoap detergents.
  • the nonionic detergents are a well-known class of low sudsing detergents and are produced by the condensation of several moles of a hydrophilic alkylene oxide, such as ethylene oxide or propylene oxide, with a hydrophobic base, such as an alkylated phenol, a fatty alcohol, a fatty amine, a fatty amide, or the hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
  • the alkyl phenolalkylene oxide condensates are generally prepared by condensing one mole of an alkyl phenol having from about 9 to about carbon atoms in the alkyl radical with from about 8 to about moles of an alkylene oxide, such as ethylene oxide or propylene oxide.
  • condensation product of one mole of dodecyl phenol With an average of 10 moles of ethylene oxide sold commercially under the name Sterox DI the condensation product of 1 mole of nonyl phenol with an average of 9 moles of ethylene oxide sold commercially under the name Igepal (IO-630, the condensation product of 1 mole of nonyl phenol With an average of 10 moles of ethylene oxide sold commercially under the name "I'ergitol NPX, and the condensation product of 1 mole of nonyl phenol with an average of 20 moles of ethylene oxide sold commercially under the name Igepal CO- 850.
  • nonionic detergents which are condensation products of a fatty alcohol With an alkylene oxide is the condensate of 1 mole of tridecyl alcohol With an average of 10 moles of ethylene oxide sold commercially under the name Stereox AJ-100.
  • Condensates of tall oil with alkylene oxides also form nonionic detergents. Typical of these is the condensate of 1 mole of tall oil with an average of 10 moles of ethylene oxide sold commercially under the name Sterox CD.
  • the polyoxyalkylene alkanols are also nonionic detergents and are made by the condensation of an alkylene oxide with a hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
  • These nonionic detergents which are described in US. Patent No. 2,674,619 and are sold under the name Pluronic, have the following empirical formula
  • the hydrophobic base portion of this nonionic detergent i.e., the (C H O) portion, generally has a molecular Weight from 801 to 2100.
  • the amount of ethylene oxide in these compounds is represented by the sum of a plus 0 which is an integer such that the molecule contains from 0 to 90% of ethylene oxide.
  • Pluronic L-60 b represents a molecular weight of 1501 to 1800 and a plus 0 is an integer such that the molecule contains 0-10% ethylene oxide.
  • Pluronic L-61 [2 represents a molecular weight of 1501-1800 and a plus c is an integer such that the molecule contains 10 to 20% ethylene oxide.
  • Pluronic L-64 b represents a molecular weight of 1501- 1800 and a plus c is an integer such that the molecule contains 40-50% ethylene oxide.
  • Pluronic F-38 b represents a molecular weight of 801-1000 and a plus 0 is an integer such that the molecule contains 80-90% ethylene oxide.
  • Pluronic F-68 b represents a molecular weight of 1501-1800 and a plus 0 is an integer such that the molecule contains 80-90% ethylene oxide.
  • Pluronic P-75 [1 represents a molecular weight of 1801- 2100 and a plus 0 is an integer such that the molecule contains 50-60% ethylene oxide.
  • Suitable nonionic detergents are the diethanolamides of long chain fatty acids, such as lauric diethanolamide.
  • the phosphate component of the detergent briquettes is present therein in an amount from about 20% to about 95% by Weight, and preferably in an amount of about 60% by weight. This amount of phosphate substantially prevents bleeding or oiling out or separation from the tablets of any normally liquid or oily nonionic detergent present therein. The lower the level of normally liquid or oily nonionic detergent present, the less phosphate is needed to prevent bleeding.
  • the phosphate can be tetrapotassium pyrophosphate, or pentasodium or pentapotassium tripolyphosphate.
  • the tripolyphosphate as used can be completely anhydrous or the commercial anhydrous variety containing small amounts of water, either uncombined or in the form of small amounts of tripolyphosphate hexahydrate, up to, for example, about 1%.
  • sodium tripolyphosphate When sodium tripolyphosphate is used, it may be type II (wherein the tripolyphosphate content contains at least 95% Form II), or if rapid disintegration as well as rapid solubility is desired, it must be a mixture of Form I and Form II in which one form may vary from 10% to 90%, and the other from 90% to 10% respectively, in order for the resulting detergent tablets to have a high rate of disintegration, even in unagitated water, as Well as rapid solubility in water. Commercial type I sodium tripolyphosphate containing about 20% Form I and Form II is suitable. Detergent tablets prepared from completely anhydrous or commercial anhydrous type II sodium tripolyphosphate have extremely slow disintegration rates but acceptable solubility rates.
  • Detergent tablets prepared by using a tripolyphosphate which is entirely in the hexahydrate form are unsatisfactory, because such tablets have an extremely poor rate of disintegration and solubilization.
  • a portion of the tetrapotassium pyrophosphate or pentasodium or pentapotassium tripolyphosphates can be substituted by other phosphates.
  • the relative amounts of phosphate and nonionic detergent are also critical.
  • the weight rat-i0 of phosphate to nonionic detergent lies in the range from about 2:1 to about 20:1, and preferably is about 6:1.
  • the detergent tablets can contain other components in addition to the essential phosphate and nonionic detergent components.
  • the detergent briquettes contain one or more inorganic builder salts such as alkali metal, e.g., potassium or sodium, sulfate, carbonate and silicate.
  • the builder component can be present in an amount from about 0.25% to about 70% by weight, although it is preferred to use from about 19% to about 30% by weight thereof. It is particularly preferred to use about 6% by weight of alkali metal silicate and about 15% by weight of alkali metal sulfate as the builder.
  • a further optional component in the detergent tablets is water which can be present in an amount up to about by Weight in order to facilitate the preparation of the tablets.
  • Other optional components include fluorescent dyes or optical brighteners, soil suspending agents, perfumes, water dispersible colorants or pigments or dyes, and the like which are generally present in a small amount up to about 1% by weight.
  • a silicate is used to inhibit bleeding, the blending is performed by adding the nonionic detergent to the phosphate and then adding the silicate thereto.
  • the water dispersible colorant or pigment or dye is added to the silicate (rather than to the nonionic detergent) prior to adding the silicate to the nonionic detergent and the phosphate.
  • This blending can be readily achieved in a rotary mixer. It is preferred that one or more of the components in the mixture be in a liquid or paste state in order to facilitate agglomeration.
  • the resulting granules are screened by passing the granules through an 8-10 mesh screen.
  • the resulting uniform mixture is compressed into the shape of tablets.
  • the ultimate shape can be any suitable one, such as cylindrical, hexagonal, square, cylindrical with truncated faces, etc.
  • the amount of pressure necessary to compress the mixture into tablet form will, of course, vary with the nature, physical state, total amounts and relative amounts of the components present in the mixture. In general, however, the mixture is compressed into tablets at a pressure ranging from 200 to 5000 pounds per square inch, and usually at a pressure from 500 to 1500 pounds per square inch.
  • the resulting tablets or briquettes can be further treated, if desired, to improve the properties thereof.
  • the surface of the tablets can be moistened with from 0.1% to 0.4% by weight of water.
  • the water can be in the form of steam, water spray, or humid atmosphere.
  • the moistening of the tablet surface does not appreciably change the fracture strength of the tablets, but it does increase the surface hardness, abrasion resistance and surface smoothness of the tablets.
  • the amount of water used in moistening the surface of the tablets is critical, because the use of 0.5% or more by weight of water on the tablet surfaces causes the surface to swell and pull away from the body of the tablets and thereby form a very fragile shell.
  • This shell is very easily cracked and flakes away from the tablet leaving a core of untreated tablet which generally lacks suflicient abrasion resistance. This does not lessen friability but rather increases it. Moreover, the use of 0.5% or more by weight of water in the surface moistening treatment may also cause unsightly protuberances to appear on the surface of the tablets.
  • the pellets are aged for a time up to 8 hours or longer after the moistening treatment to harden the surface of the pellets.
  • This ageing can be performed at room temperature or higher, although the ageing temperature should not be so high as to have a deleterious effect on any of the components in the tablet, such as any perfume which might be present therein.
  • This improvement comprises chilling the tablets, either with or without prior surface moistening, to accelerate the strengthening thereof so that the handling and packaging of the tablets without crumbling is facilitated and the production rate is increased considerably.
  • the chilling can be done by exposing the tablets to substantially quiescent or moving cold air for a short period of time. In general the time of chilling can be decreased as the temperature of the cold air is lowered or as the velocity of the cold air is increased.
  • the strengthening of the tablets can be accelerated by chilling them at a temperature not substantially above 45 F. for at least about 5 minutes. Typical conditions using substantially quiescent cold air are a temperature from about 10 F.
  • Representative conditions using moving cold air are an air velocity of from about 1 foot per second to about 15 feet per second, an air temperature from about 30 F. to about 45 F. and an exposure time from about 10 minutes to about 20 minutes.
  • the process of the present invention is also applicable to the strengthening of detergent tablets or briquettes wherein the total and relative amounts of phosphate and nonionic detergent differ from those necessary in the above described Black and Gray process. Furthermore, it can be applied to the strengthening of high sudsing detergent tablets containing the well known synthetic organic anionic nonsoap detergents, e.g., the alkylarylsulfonates. The following two formulations are representative thereof.
  • chilling is performed by exposing the compressed tablets to air moving at a velocity of from about 1 foot per second to about 15 feet per second and having a temperature from about 30 F. to about 45 F. for from about 10 minutes to about 20 minutes.
  • chilling is performed by exposing the surface-moistened compressed tablets to air moving at a velocity of from about 1 foot per second to about 15 feet per second and having a temperature from about 30 F. to about 45 F. for from about 10 minutes to about 20 minutes.

Landscapes

  • 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)
US183021A 1962-03-28 1962-03-28 Process for preparing detergent tablets Expired - Lifetime US3344076A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CA733929A CA733929A (en) 1962-03-28 Detergent tablets
US183021A US3344076A (en) 1962-03-28 1962-03-28 Process for preparing detergent tablets
FR929480A FR1357206A (fr) 1962-03-28 1963-03-27 Pains de détergent
BE646800A BE646800A (en:Method) 1962-03-28 1964-04-20

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US183021A US3344076A (en) 1962-03-28 1962-03-28 Process for preparing detergent tablets

Publications (1)

Publication Number Publication Date
US3344076A true US3344076A (en) 1967-09-26

Family

ID=22671091

Family Applications (1)

Application Number Title Priority Date Filing Date
US183021A Expired - Lifetime US3344076A (en) 1962-03-28 1962-03-28 Process for preparing detergent tablets

Country Status (4)

Country Link
US (1) US3344076A (en:Method)
BE (1) BE646800A (en:Method)
CA (1) CA733929A (en:Method)
FR (1) FR1357206A (en:Method)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4077890A (en) * 1973-02-23 1978-03-07 Graham Barker Composition for treating fabrics, method for making and using the same
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4253842A (en) * 1974-05-15 1981-03-03 Colgate-Palmolive Company Detergent compositions and washing methods including and utilizing separate tablets of components
US4370250A (en) * 1976-12-06 1983-01-25 Colgate-Palmolive Company Detergent tablet
US4451386A (en) * 1976-12-06 1984-05-29 Colgate-Palmolive Company Detergent tablet
US4915862A (en) * 1988-08-11 1990-04-10 The Procter & Gamble Company Granular detergent compositions containing crutched and admixed phosphate builder system
US5133892A (en) * 1990-10-17 1992-07-28 Lever Brothers Company, Division Of Conopco, Inc. Machine dishwashing detergent tablets
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
US5571287A (en) * 1993-01-11 1996-11-05 Colgate-Palmolive Company Soap composition containing sodium pyrophosphate
US6497157B1 (en) * 1999-11-29 2002-12-24 Distek, Inc. Intrinsic dissolution apparatus with stationary sample holder

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2875155A (en) * 1954-12-09 1959-02-24 Colgate Palmolive Co Detergent briquette and process for the production thereof
US2961410A (en) * 1957-04-02 1960-11-22 Procter & Gamble Process for preparing detergent compositions
US3081267A (en) * 1959-12-31 1963-03-12 Procter & Gamble Detergent tablet and process for making same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2875155A (en) * 1954-12-09 1959-02-24 Colgate Palmolive Co Detergent briquette and process for the production thereof
US2961410A (en) * 1957-04-02 1960-11-22 Procter & Gamble Process for preparing detergent compositions
US3081267A (en) * 1959-12-31 1963-03-12 Procter & Gamble Detergent tablet and process for making same

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4077890A (en) * 1973-02-23 1978-03-07 Graham Barker Composition for treating fabrics, method for making and using the same
US4253842A (en) * 1974-05-15 1981-03-03 Colgate-Palmolive Company Detergent compositions and washing methods including and utilizing separate tablets of components
US4370250A (en) * 1976-12-06 1983-01-25 Colgate-Palmolive Company Detergent tablet
US4451386A (en) * 1976-12-06 1984-05-29 Colgate-Palmolive Company Detergent tablet
US4219436A (en) * 1977-06-01 1980-08-26 The Procter & Gamble Company High density, high alkalinity dishwashing detergent tablet
US4915862A (en) * 1988-08-11 1990-04-10 The Procter & Gamble Company Granular detergent compositions containing crutched and admixed phosphate builder system
US5133892A (en) * 1990-10-17 1992-07-28 Lever Brothers Company, Division Of Conopco, Inc. Machine dishwashing detergent tablets
US5571287A (en) * 1993-01-11 1996-11-05 Colgate-Palmolive Company Soap composition containing sodium pyrophosphate
US5552079A (en) * 1993-09-13 1996-09-03 Diversey Corporation Tableted detergent, method of manufacture and use
US6497157B1 (en) * 1999-11-29 2002-12-24 Distek, Inc. Intrinsic dissolution apparatus with stationary sample holder

Also Published As

Publication number Publication date
BE646800A (en:Method) 1964-10-20
FR1357206A (fr) 1964-04-03
CA733929A (en) 1966-05-10

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