US3030312A - Detergent composition - Google Patents

Detergent composition Download PDF

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Publication number
US3030312A
US3030312A US304853A US30485352A US3030312A US 3030312 A US3030312 A US 3030312A US 304853 A US304853 A US 304853A US 30485352 A US30485352 A US 30485352A US 3030312 A US3030312 A US 3030312A
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US
United States
Prior art keywords
detergent
methyl sulfate
caking
alkyl
sodium
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
US304853A
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English (en)
Inventor
Mills Victor
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
Original Assignee
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
Family has litigation
Priority to BE522112D priority Critical patent/BE522112A/xx
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=23178279&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=US3030312(A) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Priority to US304853A priority patent/US3030312A/en
Priority to GB22662/53A priority patent/GB739817A/en
Priority to DEP10297A priority patent/DE935207C/de
Application granted granted Critical
Publication of US3030312A publication Critical patent/US3030312A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/37Mixtures of compounds all of which are anionic
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/34Organic compounds containing sulfur
    • C11D3/3409Alkyl -, alkenyl -, cycloalkyl - or terpene sulfates or sulfonates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols

Definitions

  • this invention relates to wetting, sudsing and detergent compositions in small solid particle form, such as spray-dried granules, which have improved anti-caking properties.
  • a number of synthetic detergent products when in small solid particle form exhibit the very undesirable tendency to lose their free-flowing properties and cake or form lumps while in storage on the retail dealers shelves. This tendency is particularly apparent in products containing Water soluble salts of alkyl aryl sulfonic acids, such as, for example, sodium alkyl benzene sulfonate, whether the alkyl aryl sulfonate comprises the sole active ingredient of the detergent composition or is in admixture with various other types of synthetic organic detergents, the mixture comprising the active portion of the detergent composition.
  • This caking and lumping tendency is enhanced by the presence of atmospheric heat and moisture and therefore such products tend to lose their free-flowing characteristics much more readily while in storage under conditions prevailing during the summer months.
  • amounts of the methyl sulfate salt equivalent to about 2% to about 6% by weight of the final detergent product amounts less than 2%, for example, about 1.5%, may be used to advantage.
  • amounts in excess of 6%, for example, up to about 10% may be employed without undue v adverse effects. Amounts in excess of 10% may be used but there is no apparent advantage in using such greater amounts. In fact, some undesirable effects, such as a decrease in detergency, have been noted when such larger quantities are present in the detergent. product.
  • methyl sulfate may also be realized from the incorporation of methyl sulfate into such products.
  • the neutralized mixture when sodium hydroxide or a sodium salt is used as the neutralizing agent, comprises a substantial percentage of sodium sulfate. This salt contributes little if anything of value to the finished prod- 3&30312 Patented Apr.
  • the neutralized reaction mixture referred to above is normally mixed with various other materials which may be desirably present in such products, e.g. inorganic builders like the alkali metal phosphates, silicates and carbonates and organic additives like carboxymethyl cellulose, higher fatty alcohols and various amides, and this mixture is then subjected to a spray-drying operation as is well known in the art.
  • inorganic builders like the alkali metal phosphates, silicates and carbonates and organic additives like carboxymethyl cellulose, higher fatty alcohols and various amides
  • this mixture is then subjected to a spray-drying operation as is well known in the art.
  • a typical spray-drying operation such a mixture is first prepared in a flowing condition which is referred to in the art as a paste.
  • This paste is then pumped through a spray nozzle which atomizes it into the upper part of a chamber or tower containing a column of air which has been heated to a temperature in the range from about 2 0-500 F. and which may pass in either concurrent or countercurrent direction to the sprayed mixture to evaporate the water from the falling atomized particles.
  • My invention is not limited to any particular method of incorporating the methyl sulfate into the detergent compositions and any satisfactory method may be used.
  • the methyl sulfate may be crutched into the detergent mixture when it is in paste form just prior to spray-drying or it may be added according to the metl 0d outlined in the Korpi and Whyte application, SN. 289,434, filed May 22, 1952, now Patent No. 2,742,435.
  • the active ingridents comprise a mixture of an alkyl benzene sulfonate and an alkyl sulfate, the alkyl chains in each case containing from eight to about twenty-two carbon atoms).
  • detergent compositions having from about 15% to about 95% of alkyl aryl sulfonate as an active organic detergent ingredient may be improved as to anti-caking properties by means of my invention.
  • my invention may be advantageously employed with highly built" detergent compositions which contain a water soluble salt of an alkyl aryl sulfonic acid as an active ingredient and which exhibit the caking and lumping tendency as well as with those compositions wherein such organic detergent ingredient comprises a major portion of the detergent composition.
  • those detergent compositions which contain at least 15% by weight of an alkyl aryl sulfonate as the active organic detergent ingredient and sodium tripolyphosphate as a builder, and in which the ratio of sodium tripolyphosphate to the active organic detergent ingredient varies from about 1:1 to about :1 are benefitted by my invention.
  • a method of determining the caking values of the various detergent products in small particle form is set forth immediately below.
  • the test is normally run under rather drastic conditions of temperature and humidity which promote the tendency of the products to cake and lump. This is to simulate the storage conditions the product is subjected to on the retailers shelves during the summer months. It is to be understood of course that, if desired, other conditions of temperature and humidity may be used in the testing procedure.
  • Samples to be tested are packaged as they would be for normal retail use, i.e., in cartons which have received no special moisture-proofing treatment, and are then placed in a cabinet in which air of fixed temperature and humidity (e.g. 90 F. at 80% relative humidity) is circulated. After storage for varying lengths of time, depending upon the storage conditions which are to be simulated, the samples are graded according to the ease with which they pour from the carton, the amount of product present in the form of lumps and the amount of product which is hung-up on the sides of the carton. The samples may be either poured from the carton by hand or, to eliminate the possibility of human error, by machine.
  • air of fixed temperature and humidity e.g. 90 F. at 80% relative humidity
  • the grading scale covers the range from O to 100, a grade of 0 representing a product that cannot be removed from the carton without tearing the carton open and a grade of 100 representing a product that pours like dry sand.
  • the actual grade is the amount of the product in terms of percent, based on the total amount of product in the carton, which will pour out and pass through a wire screen having a inch mesh.
  • Example 1 Two samples of a spray-dried detergent composition were prepared.
  • the active ingredient of each sample was principally dodecyl benzene sulfonate and comprised about 26% by weight of the composition.
  • the remainder of the detergent composition comprised essentially sodium sulfate along with other additives in minor amounts.
  • One sample contained 4% sodium methyl sulfate by weight of the product as a caking inhibiting agent and the other sample contained no sodium methyl sulfate.
  • Example 2 --Two samples of a spray-dried composition containing an alkyl benzene, the alkyl chain of which contained an average of about 12 carbon atoms, in an amount equal to about 26% by weight of the detergent composition, as the active ingredient were prepared. The remainder of the composition comprised essentially sodium sulfate along with other additives in minor amounts. One of the samples contained about 2% by weight of sodium methyl sulfate and the other sample contained no sodium methyl sulfate and was used as a blank for comparison purposes. These products were packed into paperboard cartons as specified in Example 1, and their caking values were determined after storage for varying lengths of time at 90 F. and 80% relative 1 Coking value before storing under conditions specified.
  • Example 3 Two samples of a spray-dried detergent composition, containing about 26% active ingredient, 75% of which was an alkyl benzene sulfonate and 25% of which was an alkyl sulfate whose alkyl chain was obtained from the high molecular weight fatty alcohols derived from coconut oil, were prepared. The remainder of the detergent composition comprised essentially sodium sulfate along with other additives in minor amount. One sample contained 4% sodium methyl sulfate as a caking inhibitor and the other sample, containing no sodium methyl sulfate, was used as a blank for comparison purposes.
  • Example 4 A sample of a spray-dried detergent composition was prepared which contained, as the active ingredient, 18.3% by weight of an alkyl benzene sulfonate, the alkyl chain of which contained an average of about 12. carbon atoms, 44.5% sodium tripolyphosphate, and 4% sodium methyl sulfate as the caking inhibitor, as well as other minor constituents.
  • any water-soluble salt of methyl sulfate such as, for example, the magnesium or potassium salts, may be substituted for sodium methyl sulfate with comparable results.
  • a wetting, sudsing and detergent composition in small solid particle form which comprises a mixture of an organic detergent agent, selected from the group consisting of water soluble salts of alkyl substituted mononuclear aryl sulfoni: acids and mixtures thereof with water soluble salts of alkyl sulfuric acid esters, all containing from 8 to 22 carbon atoms in the alkyl chain, the said organic detergent agent being characterized by its tendency to promote caking in detergent compositions and a water soluble salt of methyl sulfate in an amount at least 1.5% by weight of the detergent composition and sufi'icient to inhibit the caking thereof.
  • an organic detergent agent selected from the group consisting of water soluble salts of alkyl substituted mononuclear aryl sulfoni: acids and mixtures thereof with water soluble salts of alkyl sulfuric acid esters, all containing from 8 to 22 carbon atoms in the alkyl chain, the said organic detergent agent being characterized by its tendency to promote caking in detergent
  • organic detergent agent is a water soluble salt of an alkyl benzene sulfonate, the alkyl chain of which contains from 8 to 22 carbon atoms.
  • a wetting, sudsing, and detergent composition in small solid particle form which comprises a mixture of an organic detergent agent selected from the group consisting of water-soluble salts of alkyl substituted mononuclear aryl sulfonic acids and mixtures thereof with water-soluble salts of alkyl sulfuric acid esters, the alkyl chain in each case containing from 8 to 22 carbon atoms, the said organic detergent agent being characterized by its tendency to promote caking in detergent compositions,
  • organic detergent agent a sodium alkyl substituted mononuclear aryl sulfonate, the alkyl chain of which contains from 8 to 22 carbon atoms, the said organic detergent agent being characterized by its tendency to promote caking in detergent compositions, and a caking inhibiting amount of a water-soluble salt of methyl sulfate.

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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)
  • Detergent Compositions (AREA)
US304853A 1952-08-16 1952-08-16 Detergent composition Expired - Lifetime US3030312A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BE522112D BE522112A (en)) 1952-08-16
US304853A US3030312A (en) 1952-08-16 1952-08-16 Detergent composition
GB22662/53A GB739817A (en) 1952-08-16 1953-08-17 Detergent compositions
DEP10297A DE935207C (de) 1952-08-16 1953-08-18 Netz-, Wasch- und Reinigungsmittel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US304853A US3030312A (en) 1952-08-16 1952-08-16 Detergent composition

Publications (1)

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US3030312A true US3030312A (en) 1962-04-17

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US304853A Expired - Lifetime US3030312A (en) 1952-08-16 1952-08-16 Detergent composition

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BE (1) BE522112A (en))
DE (1) DE935207C (en))
GB (1) GB739817A (en))

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3256202A (en) * 1964-06-01 1966-06-14 Alcolac Chemical Corp Surface-active agents and detergent compositions
US3303136A (en) * 1963-02-26 1967-02-07 Lever Brothers Ltd Detergent compositions
WO1993012216A1 (de) * 1991-12-17 1993-06-24 Henkel Kommanditgesellschaft Auf Aktien GRANULAT, ENTHALTEND α-SULFOFETTSÄUREALKYLESTER

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2631980A (en) * 1949-07-22 1953-03-17 California Research Corp Noncaking alkyl aryl sulfonate detergent compositions
US2742435A (en) * 1952-05-22 1956-04-17 Procter & Gamble Process for preparing detergent compositions

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2631980A (en) * 1949-07-22 1953-03-17 California Research Corp Noncaking alkyl aryl sulfonate detergent compositions
US2742435A (en) * 1952-05-22 1956-04-17 Procter & Gamble Process for preparing detergent compositions

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3303136A (en) * 1963-02-26 1967-02-07 Lever Brothers Ltd Detergent compositions
US3256202A (en) * 1964-06-01 1966-06-14 Alcolac Chemical Corp Surface-active agents and detergent compositions
WO1993012216A1 (de) * 1991-12-17 1993-06-24 Henkel Kommanditgesellschaft Auf Aktien GRANULAT, ENTHALTEND α-SULFOFETTSÄUREALKYLESTER

Also Published As

Publication number Publication date
GB739817A (en) 1955-11-02
DE935207C (de) 1955-11-17
BE522112A (en))

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