US3330766A - Discoloration inhibitors - Google Patents

Discoloration inhibitors Download PDF

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Publication number
US3330766A
US3330766A US499082A US49908265A US3330766A US 3330766 A US3330766 A US 3330766A US 499082 A US499082 A US 499082A US 49908265 A US49908265 A US 49908265A US 3330766 A US3330766 A US 3330766A
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United States
Prior art keywords
manganese
detergent
solution
cerium
water
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Expired - Lifetime
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US499082A
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English (en)
Inventor
Goldwasser Seymore
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Lever Brothers Co
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Lever Brothers Co
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Priority to US499082A priority Critical patent/US3330766A/en
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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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/046—Salts
    • 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
    • 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
    • C11D3/39—Organic or inorganic per-compounds
    • 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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-compounds
    • 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
    • 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
    • C11D3/3955—Organic bleaching agents
    • 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 to the prevention of discoloration caused by the presence of manganese ions in washing solutions, and more particularly to cleansing and bleaching compositions suitable for use in manganese containing water.
  • the need for protection against staining is particularly acute within the pH range generally encountered in cleansing and bleaching operations, that is from about 5.5 to about 10.5.
  • a further object of the invention is to provide staininhibiting compositions for use in manganese-containing solutions.
  • a still further object of the invention is to provide cleansing and bleaching compositions which are suitable for use in manganese containing water's.
  • a cleansing solution containing the stain-producing manganese ions a stain inhibiting amount of a water soluble cerium compound.
  • a stain inhibiting amount of a water soluble cerium compound a water soluble cerium compound.
  • a preferred stain inhibitor is a composition comprising both a water soluble compound capable of providing cerium ions in solution and a pyrophosphate salt such as an alkali metal pyrophosphate, e.g., sodium pyrophosphate, potassium pyrophosphate, and the like.
  • a pyrophosphate salt such as an alkali metal pyrophosphate, e.g., sodium pyrophosphate, potassium pyrophosphate, and the like.
  • the small amount of pyrophosphate e.g., about 5 percent or less, which is normally present in commercial tripolyphosphate, is sufficient to provide adequate protection.
  • As little as about 1 weight percent of pyrophosphate in a detergent formulation or about 20-30 parts per million in the cleansing solution is effective to promote the stain inhibitingqualities of cerium ions.
  • inhibiting amount and effective amount refer to that amount of the inhibitor which is to be added to the manganese-containing cleansing solution in order to provide the desired degree of stain inhibition when used in accordance with the manufacturers directions, as for example, in a textile wash solution, a bleaching bath or a dishwashing solution.
  • Cerium ions for use in the practice of the instant invention may be provided by the use of water-soluble cerium compounds.
  • Illustrative water-soluble cerium compounds include ceric nitrate, cerous acetate, cerous bromate, cerous bromide, cerous chloride, cerous nitrate, cerous sulfate, and the like or mixtures of rare earth salts containing cerium compounds.
  • Cerium oxide while normally considered to be insoluble in Water, has been found to be effective when added to a detergent composition and admixed therewith, e.g., in a soap crutcher, at an elevated temperature in the presence of polyphosphates and'a relatively high alkalinity (pH about 10), and accordingly is considered to be within the scope of the term water-soluble, which term is intended to describe any compound which is capable of providing the inhibitor concentration levels which are necessary for the prevention or diminution of manganese staining.
  • the herein disclosed inhibitors have been found to be effective in inhibiting manganese staining caused by manganese ions in the presence of bleaching agents capable of oxidizing manganese ions to a higher valence state such as halogen containing bleaching agents, e.g., potassium and sodium dichlorocyanurate, dichloroisocyanuric acid, trichlorocyanuric acid, dichlorodimethylhydantoin, N,N-dichloro-p-toluenesulfonamide, sodium chlorite, sodium and potassium hypochlorite and oxygen releasing bleaching agents, e.g., hydrogen peroxide, lauryl peroxide, potassium and ammonium monopersulfate, sodium perborate, sodium pyrophosphate peroxide and the like.
  • bleaching agents capable of oxidizing manganese ions to a higher valence state
  • bleaching agents capable of oxidizing manganese ions to a higher valence state
  • bleaching agents capable
  • the actual amount of the inhibitor which is necessary to provide adequate protection depends on a number of conditions, e.g., the concentration of the manganese ions,
  • the discoloration inhibitor can be added to or incorporated into the cleansing solution in a variety of ways. They may be formulated into dry or liquid detergent formulations, detergent-bleach formulations or bleach formulations for concurrent addition to the cleansing solution. For example, they may be conveniently admixed with synthetic detergent formulations containing one or more anionic or nonionic detergents in combination with inorganic builders such as condensed inorganic polyphosphates, e.g., tripolyphosphates and pyrophosphates. Alternatively, they may be packaged separately in liquid or dry form for selective addition to a Washing or bleaching bath. Since local water conditions vary and to a large extent determine the degree of staining, this procedure offers a more practical means of providing optimum inhibition under varying conditions.
  • detergents which may be present in the formulations in which the inhibitors of this invention are present include the well-known sulfated fatty alcohols, alkyl-substituted aromatic sulfonates, alkanesulfonates, hydroxyalkanesulfonate esters of aliphatic acids having about 10 to 18 carbon atoms, sulfonated fatty oils, sulfated and sulfonated alkoxy derivatives, sulfuric acid esters of monoglycerides, and taurine derivatives.
  • the alkali metal, ammonium alkyl and alkanol substituted ammonium salts of these materials are ordinarily employed in the formulation of detergents.
  • the inhibitors are also useful with nonionic detergents, such as ethoxylated alcohols, thioalcohols or acids; alkyl substituted phenols; alkylolamides of fatty acids; and nonionic detergents such as the pluronics which are polyoxypropylene polymers containing varying proportions of polyoxyethylene units in the molecule.
  • nonionic detergents such as ethoxylated alcohols, thioalcohols or acids; alkyl substituted phenols; alkylolamides of fatty acids; and nonionic detergents such as the pluronics which are polyoxypropylene polymers containing varying proportions of polyoxyethylene units in the molecule.
  • the detergent compositions can also contain builders, fillers, soil suspending agents and other conventional ingredients found in detergent formulations.
  • the formulations may be prepared by conventional methods well known in the detergent industry such as by blending the ingredients in aqueous solutions or slurries and then spray drying at elevated temperatures.
  • Swatches of white cloth were washed in a wash water containing about 0.1 part per million of manganese ions, 180 parts per million of calcium and magnesium ions in a ratio of about 2 to 1, about 0.25 weight percent of one of the detergent formulations described above, and about 200 parts per million of chlorine.
  • the cloths were washed, under conditions which simulated normal laundry procedure, in a small washing machine with the temperature of the wash solution at about F.
  • the wash procedure consisted of a Wash cycle and a fresh water rinse cycle, after which the cloths were squeeze dried.
  • the cloths were Washed a total of 10 times using each of the described detergent formulations. Reflectance measurements were made on each sample after the second, fifth, and tenth wash, using a spectrophotometer at 430 millimicrons. The reflectance for each measurement on the various formulations are given below.
  • composition Number Wash It is apparent that repeated exposure to wash water containing manganese ions and a bleaching agent has caused considerable loss of reflectance in the test performed with detergent compositions in which no inhibitor was employed, i.e., in compisition 1 above, whereas, the cloths washed with inhibitor-containing detergent formulations (composition 2 and 3) showed improved reflectance indicating substantial reduction of manganese staining after repeated washings.
  • Example 2 The following spray-dried nonionic detergent compositions were prepared:
  • Polyoxypropylenc havmg a molecular weight of from 1,500 to 1,800.
  • Example 1 The washing procedure outlined in Example 1 was followed.
  • composition 2 the detergent containing the discoloration inhibitor, i.e., composition 2, is characterized by a significantly higher reflectance than composition 1, which is a control containing no cerium. This increased reflectance indicates the substantial reduction of manganese staining on the cloths washed with the inhibitor-containing detergents.
  • Example 3 A nonionic detergent formulation as described in Example 2, above, was divided into two portions. To one portion there was added 0.1 Weight percent cerium ion in the form of cerous nitrate. The second portion was used as a control and contained no inhibitor. Pieces of cotton cloth were washed in wash water containing 0.1 part per million of manganese ion using about 0.25 weight percent of each of the above formulations under identical conditions. The washing was conducted in two series. In one series about 200 parts per million of chlorine was added to the wash solution. In the second series no bleaching agent was used. The complete laundry cycle consisted of a fifteen minute wash period at about 120 F. followed by a three minute rinse. The laundry cycle was repeated times and reflectance measurements were made after the second, fifth, and tenth wash. The results are tabulated below:
  • This example illustrates the ability of cerium ions to prevent or diminish the discoloration of textile surfaces caused by the simultaneous presence of manganese ion and a bleaching agent.
  • Example 4 Four solutions as shown below, were prepared from water containing 3 parts per million (p.p.m.) of manganese ion and 200 parts per million of chlorine in the form of sodium hypochlorite:
  • Solution Number Cloth Type This example shows that discoloration occurs when manganese ions and bleach are present even in the absence of organic detergents and that cerium ion is effective as a manganese-stain inhibitor even in the absence of organic detergents.
  • the sample to be tested was weighed into a marked 250 ml. Pyrex beaker, a platinum strip approximately 15 mm. x 15 mm. x 0.003 inch was suspended therein and about 200 m1.
  • Water containing manganese ion pre-heated to F. was added.
  • the beaker containing the test solution and the platinum strip was then put into a water bath maintained at a temperature of about 143 F. After vigorous initial stirring to dissolve the sample, the test solution was agitated at frequent intervals.
  • Several samples and a control were tested simultaneously and test solutions and platinum strips were observed closely for discoloration and other changes. Fifteen minutes after the addition of the water containing manganese ion, the platinum strips were removed from the solutions and examined.
  • the strips were compared and graded against a control and were reintroduced into the solutions for an additional fifteen minute period. After a total exposure period of about thirty minutes, the platinum strips were again removed from the solution and examined, compared and graded. In certain cases, this procedure was varied to extend the total exposure period of the strips to more than thirty minutes.
  • Example 6 The following dishwashing formulation of a conventional type was used in the test described above:
  • Chlorinating agent to yield 0.9%1% available chlorine, based on total formula weight.
  • chlorina'ting agents were employed: potas sium dichlorocyanurate, dichloroisocyanuric acid, diehlorodimethylhydantoin, sodium chlorite, chlorine gas bubbled into solution, N,N-diohloro-ptoluenesulfonamide, sodium dichloroisocyanurate and trichloroisocyanuric acid.
  • test solution consisted of 200 ml. of water containing 5 ppm. of Mn++ (143145 F.) and a sufiicient 4 amount of the above detergent to form a 0.25% solution.
  • Mn++ 143145 F.
  • sufiicient 4 amount of the above detergent to form a 0.25% solution.
  • Percent inhibitor (basis dry formula Platinum discoloration after contact period of- No appreciable increase in discoloring after 1.5 hr. contact period.
  • Example 7 The above described tests were conducted with aqueous solutions containing ppm. Mn++ and cerium nitrate or cerium chloride. These inhibitors in levels below about 0.5% (based on dry formula weight) proved to be mildly effective in retarding platinum discoloring. Complete inhibition of discoloration during a minute contact period was effected at a cerium nitrate level of about 2%. This level however, did not completely prevent discoloration at contact periods greater than 15 minutes.
  • a detergent composition consisting essentially of an effective amount of a manganese stain inhibiting water soluble cerium compound and a synthetic nonsoap detergent.
  • a detergent composition consisting essentially of a synthetic non-soap detergent, an alkali metal pyrophosphate salt, and an effective amount of a manganese stain inhibiting water soluble cerium compound.
  • a detergent composition consisting essentially of a synthetic non-soap detergent, an alkali metal pyrophosphate salt, an effective amount of a manganese stain inhibiting water soluble cerium compound and a bleaching agent capable of oxidizing manganese.
  • a detergent composition consisting essentially of a synthetic non-soap detergent, a bleaching agent capable of oxidizing manganese and an effective amount of a manganese stain inhibiting water soluble cerium compound.
  • composition of claim 3 wherein the bleaching agent is a halogen releasing bleaching agent.
  • composition of claim 3 wherein the bleaching agent is an oxygen releasing bleaching agent.
  • a method of inhibiting surface discoloration caused by the presence in a solution of manganese ions and a bleaching agent capable of oxidizing manganese which comprises adding to the solution a discoloration inhibiting amount of water soluble cerium compound.
  • a method of inhibiting surface discoloration caused by the presence of manganese ions and a bleaching agent capable of oxidizing manganese in a cleansing solution which comprises adding to the solution effective amounts of a water soluble cerium compound and an alkali metal pyrophosphate.
  • a method of preventing the discoloration of textile surfaces in cleansing solutions containing manganese ions and a bleaching agent capable of oxidizing manganese which comprises the addition of at least about 0.5 part per million of cerium ion to the solution.
  • An aqueous washing and bleaching solution consisting essentially of a bleaching agent, a synthetic detergent, and at least about 0.5 part per million of cerium ion.
  • a method of inhibiting the discoloration of hard surfaces exposed to an aqueous solution containing manganese ions and a bleaching agent capable of oxidizing manganese which comprises adding a discoloration inhibiting amount of a material consisting essentially of an alkali metal pyrophosphate salt and a water soluble cerium compound to said solution.
  • a composition consisting essentially of an alkali metal pyrophosphate salt and a manganese stain inhibiting amount of at least one compound which furnishes cerium ion in aqueous solution, said composition being effective to inhibit discoloration of hard surfaces exposed to a soluton containing manganese ion and a bleaching agent capable of oxidizing manganese when said composition is added to said solution.
  • a method of inhibiting the discoloration of hard surfaces which occurs in solutions containing manganese ion and a. halogen containing bleaching agent capable of oxidizing manganese which comprises adding at least about 5 parts per million of cerium ion and from about 20 to about 30 parts per million of an alkali metal pyrophosphate salt to said solution.
  • a composition for use in preventing manganese staining of hard surfaces and textiles being Washed in a solution containing manganese ions and a bleaching agent capable of oxidizing the manganese ions said composition consisting essentially of a water-soluble inert filler and an effective amount of at least one manganese stain inhibiting water-soluble cerium compound.

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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)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
US499082A 1963-11-08 1965-10-20 Discoloration inhibitors Expired - Lifetime US3330766A (en)

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US32253663A 1963-11-08 1963-11-08
US499082A US3330766A (en) 1963-11-08 1965-10-20 Discoloration inhibitors

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US (1) US3330766A (en(2012))
AT (1) AT256294B (en(2012))
BE (1) BE655438A (en(2012))
FR (1) FR1415083A (en(2012))
NL (1) NL6412998A (en(2012))

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3461202A (en) * 1966-07-28 1969-08-12 Olin Mathieson Composition and process
US4051055A (en) * 1976-12-21 1977-09-27 The Procter & Gamble Company Cleansing compositions
US5622646A (en) * 1994-04-07 1997-04-22 The Procter & Gamble Company Bleach compositions comprising metal-containing bleach catalysts and antioxidants

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2689225A (en) * 1954-09-14 Detergent compositions
US2802786A (en) * 1954-06-18 1957-08-13 Exxon Research Engineering Co Emulsifiable oil composition
US2895050A (en) * 1956-04-30 1959-07-14 Dentists Supply Co Fluorescent artificial teeth
US3049495A (en) * 1959-07-01 1962-08-14 Du Pont Peroxymonosulfate-diethylenetriamine pentaacetic acid composition
US3079347A (en) * 1960-10-25 1963-02-26 Bell Telephone Labor Inc Terbium and cerium activated calcium fluoride optical maser material
US3100683A (en) * 1962-07-18 1963-08-13 Francis P Roberts Adsorption of cerium values from aqueous solutions
US3112274A (en) * 1959-11-24 1963-11-26 Procter & Gamble Process for making a bleach composition

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2689225A (en) * 1954-09-14 Detergent compositions
US2802786A (en) * 1954-06-18 1957-08-13 Exxon Research Engineering Co Emulsifiable oil composition
US2895050A (en) * 1956-04-30 1959-07-14 Dentists Supply Co Fluorescent artificial teeth
US3049495A (en) * 1959-07-01 1962-08-14 Du Pont Peroxymonosulfate-diethylenetriamine pentaacetic acid composition
US3112274A (en) * 1959-11-24 1963-11-26 Procter & Gamble Process for making a bleach composition
US3079347A (en) * 1960-10-25 1963-02-26 Bell Telephone Labor Inc Terbium and cerium activated calcium fluoride optical maser material
US3100683A (en) * 1962-07-18 1963-08-13 Francis P Roberts Adsorption of cerium values from aqueous solutions

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3461202A (en) * 1966-07-28 1969-08-12 Olin Mathieson Composition and process
US4051055A (en) * 1976-12-21 1977-09-27 The Procter & Gamble Company Cleansing compositions
US5622646A (en) * 1994-04-07 1997-04-22 The Procter & Gamble Company Bleach compositions comprising metal-containing bleach catalysts and antioxidants

Also Published As

Publication number Publication date
BE655438A (en(2012)) 1965-05-06
AT256294B (de) 1967-08-10
NL6412998A (en(2012)) 1965-05-10
FR1415083A (fr) 1965-10-22

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