US3849346A - Process for preparing granular detergent composition - Google Patents

Process for preparing granular detergent composition Download PDF

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Publication number
US3849346A
US3849346A US00260743A US26074372A US3849346A US 3849346 A US3849346 A US 3849346A US 00260743 A US00260743 A US 00260743A US 26074372 A US26074372 A US 26074372A US 3849346 A US3849346 A US 3849346A
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US
United States
Prior art keywords
weight
sodium
sulfonate
detergent composition
granules
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
US00260743A
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English (en)
Inventor
H Kuwamura
T Tamura
I Kashiwa
T Hirabayashi
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.)
Lion Fat and Oil Co Ltd
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Lion Fat and Oil Co Ltd
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
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Publication of US3849346A publication Critical patent/US3849346A/en
Assigned to LION FAT AND OIL CO., LTD., THE reassignment LION FAT AND OIL CO., LTD., THE MERGER (SEE DOCUMENT FOR DETAILS). JAPAN, EFFECTIVE JAN. 1, 1980. Assignors: LION DENTIFRICE CO., LTD., THE
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
    • C11D1/12Sulfonic 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
    • 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
    • C11D1/143Sulfonic acid esters
    • 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
    • C11D1/146Sulfuric acid esters
    • 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
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02Preparation in the form of powder by spray drying
    • 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
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/046Salts
    • 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
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/06Phosphates, including polyphosphates
    • 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
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/08Silicates

Definitions

  • This invention relates to a process for preparing a granular detergent composition by the use of spray drying techniques. More particularly, this invention relates to a process for preparing a granular detergent composition containing particles of relatively high mechanical strength which are essentially non-caking.
  • the process for preparing the granular detergent composition in accordance with this invention is characterized by spray drying a slurry of 70-40% by weight of a detergent composition containing 10-40% by weight of an anionic surface active agent having an S0 or 80., group, 15-40% by weight of sodium tripolyphosphate, 15-40% by weight of sodium silicate having a ratio of Na O to SiO of 0.5-3, 05-10% by weight of magnesium sulfate and the remainder being other additives, in 30-60% by weight of water.
  • magnesium salts of the anionic surface active agent of the tripolyphosphate, and of the silicate are formed. It is also believed that double salts of tripolyphosphoric acid and silicic acid with the magnesium ion, are formed. These magnesium compounds have a high degree of moisture retention and a high degree of hydration. A relatively large amount of water in the slurry is consequently retained by the salts.
  • the higher-er will be the concentration of the salts formed on the surface of the dried granules.
  • Sodium silicate is normally one of the more soluble components of the composition, so that usually it will be formed in a high concentration at the surface of the granules.
  • the magnesium salts and double salts due to the formation of the magnesium salts and double salts, its solubility is decreased and the concentration of silicates formed at the surfaces of the granules is considerably reduced, while the concentration of the silicate within the granules, below the surfaces, is increased. Since caking tendency in the prior art compositions is-enhanced by high silicate concentration on the surfaces of-the granules, in the present composition, caking tendency is diminished while mechanical strength is either unaffected or is enhanced.
  • magnesium chloride does not exhibit the same effect as magnesium sulfate, presumably because the rates of magnesium salt formation are substantially different, and because the solubilities of each is substantially different.
  • Magnesium chloride moreover, has a tendency of being double decomposed to form sodium chloride. Accordingly, magnesium chloride cannot be substituted for magnesium sulfate in the present invention.
  • EXAMPLES 1-2 50 parts of sodium dodecylbenzene sulfonate (40% active ingredient and 60% water) was dissolved in 15.5 parts of water and the solution was admixed with 2.5 parts of carboxymethyl cellulose. 2 parts of sodium toluene sulfonate, 40 parts of sodium disilicate (45% active ingredient), 3 parts of polyoxyethylene nonylphenyl ether (F 5), parts of a 25% magnesium sulfate aqueous solution, 25 parts of sodium tripolyphosphate, and 22 parts of sodium sulfate, while stirring to prepare a slurry.
  • the slurry was spray dried using a disc type spray drier to prepare the granular detergent composition.
  • the granular form detergents were prepared. All of the gganular detergents respectively had a specific bulk density 0 0.27.
  • the amount of perfume is shown in percent by weight to total components.
  • Suitable anionic surface active agents which may be used herein are those having an S0 or an 80.; group, such as:
  • sodium alkylaryl sulfonate C -C sodium olefin sulfonate (C -C sodium alkyl sulfonate (C -C and sodium alkyl sulfate (C C).
  • the sodium silicate should be used in amounts of from 15-40% by weight of total solids. Less than 15% results in a composition having inadequate strength properties. Greater than 40% can result in the formation of a large amount of water-insoluble material.
  • the sodium tripolyphosphate should also be used in amounts of from 15%-40% by weight. Greater than 40% is economically unadvantageous, whereas, less than 15% is generally ineffective.
  • Magnesium sulfate should be used in an amount of from 05-10% by weight based on the total solid components in the slurry. If less than 0.5% is used, sufiicient anti-caking is not obtained, whereas if greater than 10% is used, a large quantity of water-insoluble materials may be formed.
  • the granular detergent composition prepared in accordance with the process of this invention is characterized by a high degree of granule strength so that the granules are not easily crushed during package handling. Moreover, the granules do not suffer a tendency to cake even at relatively high temperatures and relatively high humidities.
  • Caking property 50 g. of sample was introduced into a cardboard (3 cm. x 8 cm.) box which had not been pre-treated for water-proofing. The packaged detergent was kept in a room of constant temperature and humidity, at 35 C. and 85% specific humidity, for 8 hours. The contents were then spread on a 12 mesh sieve. The residual caked detergent composition was measured. The caking rate was calculated by the percentage of weight of the residual composition to 50 g. of total composition. The lower the value, the higher the anti-caking property.
  • the strength of the granules was calculated as the per centage by weight of the deducted amount of the sample passing through the sieve per 50 grams of sample. The lower the value, the less crushing of granules occurred and hence the higher the strength.
  • the intensity of perfume before the test is designated as 10 and the intensity at no perfume detection is designated as 0. The higher the number, the higher the perfume retention value.
  • the resulting dry cake was in an unbroken semicircular configuration. This cake was carefully removed from the glass vessel and the surface was shaved off. A sample from the internal part of the dry cake was also taken and both samples were analyzed.
  • a process for preparing a granular detergent composition which comprises spray drying a slurry of 70-40% by weight of a mixture of 1040% by weight of an anionic surface active agent selected from the group consisting of sodium alkylaryl sulfonate (C C sodium olefin sulfonate (C -C sodium alkyl sulfonate (C -C sodium alkyl sulfate (C -C and mixtures thereof, 15- 40% by weight of sodium tripolyphosphate, 1540% by weight of sodium silicate having an Na O to SiO ratio of 0.53, 05-10% by weight of magnesium sulfate in 30 by weight of water.
  • an anionic surface active agent selected from the group consisting of sodium alkylaryl sulfonate (C C sodium olefin sulfonate (C -C sodium alkyl sulfonate (C -C sodium alkyl sulfate (C -C and mixtures thereof, 15- 40% by
  • a granular detergent composition which comprises spray dried granules formed by spray drying a slurry consisting essentially of:
  • an anionic surface active agent selected from the group consisting of sodium alkylaryl sulfonate (Cg-C1 sodium olefin sulfonate C C sodium alkyl sulfonate (C -C sodium alkyl sulfate (C -C and mixtures thereof,
  • magnesium sulfate 0.510% by weight magnesium sulfate wherein the concentration of silicate at the surface of the granules is lessthan the concentration within said granules.

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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)
  • Glanulating (AREA)
US00260743A 1971-06-30 1972-06-08 Process for preparing granular detergent composition Expired - Lifetime US3849346A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4835471A JPS5335081B1 (enrdf_load_stackoverflow) 1971-06-30 1971-06-30

Publications (1)

Publication Number Publication Date
US3849346A true US3849346A (en) 1974-11-19

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Application Number Title Priority Date Filing Date
US00260743A Expired - Lifetime US3849346A (en) 1971-06-30 1972-06-08 Process for preparing granular detergent composition

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US (1) US3849346A (enrdf_load_stackoverflow)
JP (1) JPS5335081B1 (enrdf_load_stackoverflow)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4054541A (en) * 1974-11-04 1977-10-18 Witco Chemical Corporation Spray dried alcohol ether sulfate detergent compositions
US4111853A (en) * 1976-03-08 1978-09-05 Stepan Chemical Company Particulate composition of sodium alpha olefin sulfonate and sodium silicate
EP0030859A3 (en) * 1979-12-14 1982-01-27 Unilever Plc Process for making detergent compositions
EP0040038A3 (en) * 1980-05-10 1982-01-27 The Procter & Gamble Company Granular detergent compositions
WO2006029676A1 (en) * 2004-09-13 2006-03-23 Unilever Plc Detergent compositions and their manufacture
WO2022243264A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243283A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243276A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243265A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4054541A (en) * 1974-11-04 1977-10-18 Witco Chemical Corporation Spray dried alcohol ether sulfate detergent compositions
US4111853A (en) * 1976-03-08 1978-09-05 Stepan Chemical Company Particulate composition of sodium alpha olefin sulfonate and sodium silicate
EP0030859A3 (en) * 1979-12-14 1982-01-27 Unilever Plc Process for making detergent compositions
EP0040038A3 (en) * 1980-05-10 1982-01-27 The Procter & Gamble Company Granular detergent compositions
WO2006029676A1 (en) * 2004-09-13 2006-03-23 Unilever Plc Detergent compositions and their manufacture
WO2022243264A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243283A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243276A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle
WO2022243265A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle

Also Published As

Publication number Publication date
JPS5335081B1 (enrdf_load_stackoverflow) 1978-09-25

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Date Code Title Description
AS Assignment

Owner name: LION FAT AND OIL CO., LTD., THE

Free format text: MERGER;ASSIGNOR:LION DENTIFRICE CO., LTD., THE;REEL/FRAME:003865/0888

Effective date: 19810204