EP0328190B1 - Waschmittelzusammensetzung in Teilchenform - Google Patents

Waschmittelzusammensetzung in Teilchenform Download PDF

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Publication number
EP0328190B1
EP0328190B1 EP19890200221 EP89200221A EP0328190B1 EP 0328190 B1 EP0328190 B1 EP 0328190B1 EP 19890200221 EP19890200221 EP 19890200221 EP 89200221 A EP89200221 A EP 89200221A EP 0328190 B1 EP0328190 B1 EP 0328190B1
Authority
EP
European Patent Office
Prior art keywords
particulate
mixture
fatty acids
laundry detergent
mole
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
EP19890200221
Other languages
English (en)
French (fr)
Other versions
EP0328190A3 (en
EP0328190A2 (de
Inventor
Hendrik Willem Brouwer
Machiel Goedhart
Marco Waas
Simon Willemse
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0328190A2 publication Critical patent/EP0328190A2/de
Publication of EP0328190A3 publication Critical patent/EP0328190A3/en
Application granted granted Critical
Publication of EP0328190B1 publication Critical patent/EP0328190B1/de
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
    • C11D10/00—Compositions of detergents, not provided for by one single preceding group
    • C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/06—Inorganic compounds
    • C11D9/08—Water-soluble compounds
    • C11D9/10—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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/06—Inorganic compounds
    • C11D9/08—Water-soluble compounds
    • C11D9/10—Salts
    • C11D9/12—Carbonates
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/26—Organic compounds, e.g. vitamins containing oxygen
    • C11D9/267—Organic compounds, e.g. vitamins containing oxygen containing free fatty acids
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols

Definitions

  • the present invention relates to a novel, particulate laundry detergent composition which contains no, or reduced levels of inorganic phosphate compounds. Furthermore, it relates to a particulate base material suitable for use in such detergent compositions and to a method of manufacturing this particulate base material.
  • Conventional laundry detergent compositions contain phosphate compounds, especially sodium tripolyphosphate (STP), as building agents. Owing to the negative effects of phosphates on the environment, there has been an increasing interest in developing new laundry detergent compositions which have a low or zero phosphate content. However, it has proved to be difficult to match the excellent builder properties of the phosphate-containing compositions.
  • STP sodium tripolyphosphate
  • zeolites As builder in zero-P laundry detergent formulations.
  • the application of zeolites in laundry detergent formulations has a number of drawbacks.
  • zeolites In the first place, zeolites have a tendency to cause a bad powder structure. Further more, they tend to interact with silicates which are usually present in the composition as anti-corrosion agents, and they can cause dispensing problems in the washing machine and incrustation on the washed fabrics.
  • compositions of the invention utilise acid soap both as a powder base and as a builder.
  • the composition according to the invention comprises as a first particulate material a fatty acid mixture in which up to 35 mole% may be unsaturated fatty acids, which mixture has been neutralised to an extent of 25-60 mole %, and as a second particulate material a base in an amount sufficient to render the pH of the composition at a 0.5 wt% concentration in water higher than 8.
  • detergent additives may be present, such as a bleach system, proteolytic enzymes, anti-foaming agents, optical brighteners, perfumes, anti-corrosion additives, etc.
  • the composition according to the invention exhibits very satisfactory wash performance without the need for phosphate or zeolite builders, although the presence of low levels of these materials is not prohibited and may be beneficial. Powder properties such as flow and compressibility are also excellent.
  • the particulate laundry detergent composition according to the invention preferably contains 30-80 wt.% of granular acid soap particles.
  • the acid soap is a mixture of free fatty acids and soap, or a partially neutralized mixture of fatty acids.
  • a wide range of saturated and/or unsaturated fatty acids may be used, but it was found that the powder properties of the particulate composition become less favourable at a content of unsaturated fatty acids of more than 35 mole%. More specifically, such powders tend to be sticky and are barely free- flowing.
  • the mixture of fatty acid consists essentially of 5 - 20 mole% C16-C18 unsaturated fatty acids, and 95 - 80 mole% of a mixture of C8-C14 saturated fatty acids and C16-C18 saturated fatty acids in a ratio of 3:1-1:2.
  • C8-C14 saturated fatty acids will also be referred to as laurics
  • C14-C16 saturated fatty acids as stearics
  • C16-C18 unsaturated fatty acids as oleics.
  • the C16-C18 saturated fatty acids or stearics are mainly responsible for the builder properties, while they contribute little to detergency.
  • the C16-C18 unsaturated fatty acids or oleics are important for their builder properties but especially for detergency.
  • the C8-C14 saturated fatty acids or laurics contribute both to the building and to the detergency, but their main function is to facilitate processing of the soap/fatty acid mixture, and to ensure adequate dissolution properties.
  • the laundry detergent compositions according to the present invention can be prepared by dry-mixing the various ingredients into a suitable mixture.
  • the acid soap is used in the form of a particulate material, for example, prills or noodles.
  • Particle size and shape may be chosen at will and are discussed in more detail below.
  • These acid soap particles can be prepared by dissolving a suitable amount of soap in a mixture of fatty acid in the molten state, followed by solidification and processing of the solid mass. Alternatively, they can be prepared by partial in situ saponification or neutralization of a mixture of fatty acids. In this process, a solid base material is gradually admixed with the molten fatty acid mixture.
  • Suitable basic compounds are, for example, soda ash (sodium carbonate), sodium disilicate or metasilicate, or sodium hydroxide.
  • the operating temperature required to process these mixtures increases with the fatty acid chain length and degree of neutralization, and is preferably within the range of 70-140 ° C.
  • the detergent composition of the present invention contains a particulate base in an amount sufficient to render the pH of the composition, at a 0.5 wt.% concentration in water, higher than 8.
  • a base material in principle any base can be used which can be prepared in a particulate form and which readily dissolves in water without forming precipitates with the soap fatty acid particles.
  • the same base is used as for the partial neutralization of the fatty acid mixture.
  • the laundry detergent composition according to the invention may additionally contain other detergent compounds, such as anionic and/or nonionic non-soap detergent-active compounds. These may be incorporated in the particulate acid soap base, or present as a separate ingredient.
  • the acid soap particles may contain up to 10% by weight of anionic and/or nonionic surfactant: higher levels can be detrimental to powder properties.
  • anionic or nonionic surfactants may be carried on a porous inorganic material which is admixed with the acid soap particles.
  • An example of such an adjunct is a liquid ethoxylated C13-C15 alcohol sprayed on to a Burkeite carrier. If the inorganic carrier is a basic material, the adjunct may serve as the basic component (second particulate material) of the composition.
  • a particularly preferred method of preparing acid soap particles was found to be spray-cooling. It was found thereby that particles or prills are obtained with excellent properties with regard to the dissolution rate, stability and to wash performance of the complete detergent composition.
  • prills of any desired size and bulk density can be obtained by manipulation of the process conditions. Prills of average particle size 250-1000 m and buk density 400-750 g/e are preferred for compatibility with the other solid ingredients of the compsition, so that segregation in the pack is minimised.
  • soaps as well as fatty acids may form various eutectic complexes; such complexes may also be formed between soaps and fatty acids, resulting in highly complicated phase diagrams for such mixtures.
  • This aspect is particularly relevant to the question of meeting the 35-40 °C target for the solidification temperature.
  • the relative amounts of laurics and stearics should not exceed a 1:1 ratio; nevertheless, some liquefaction at the eutectic temperature of about 33 ° C cannot be avoided.
  • the presence of some low melting laurics/stearics complex may be expected to have a favourable effect on the low temperature solubility.
  • a number of fatty acid mixtures were prepared, having the compositions shown in Table A. The mixtures were then heated and at approximately 65 ° C they began to melt. Heating was continued and after complete melting at a temperature of about 80 ° C soda ash (sodium carbonate) was gradually added in an amount of 0.1 kg/min to control the C02-evolution until the desired degree of neutralization had been reached. At the same time, the temperature was gradually raised to approximately 140°C.
  • soda ash sodium carbonate
  • the solubility was measured as follows: The rate of dissolution of the soap/fatty acid noodles was determined by monitoring the increase in conductivity resulting from dissolution of the soap part of the noodles. In this method, 3 g/I of the sample is added to 1 I demineralized water at 25 °C with continuous stirring, using a magnetic stirrer. The rate of dissolution is expressed as the time required to dissolve 50% of the soluble part of the soap/fatty acid blend (tz ) . The maximum conductivity is measured after heating to above the melting temperature of the fatty acids, followed by cooling down to ambient temperature.
  • Examples 1-3 were repeated, but instead the molten acid/soap mixtures were spray-cooled in a spray tower to form prills.
  • the spray-cooling conditions are shown in Table B.
  • the powder properties of the prills obtained are given in Table C.
  • a mixture of fatty acids was prepared, having thefollowing composition :
  • Example 7 The procedure of Example 7 was repeated, using a fatty acid mixture of the following composition :
  • the acid soap prills obtained according to Example 7 were used to formulate a complete laundry detergent composition by dry-mixing various other ingredients to the prills, such as a nonionic detergent on a Burkeite carrier, a bleach system and an enzyme.
  • composition of the complete detergent powder is given in Table E. Also shown are two commercially available laundry detergent compositions, composition B being a low-P and composition A a zero P composition, both based on zeolites.
  • the wash performance of these three compositions was established in a Zanussi ZF 822W top loading drum washing machine, using the normal 40 °C cotton cycleprogramme "C".
  • 2.5 kg clean mixed wash load of clean cotton pieces and standard soiled test cloths was processed at a liquor/cloth ratio of approximately 6.
  • the water temperature was 20°C at a pressure of 2.0 kg/cm2.
  • the water hardness was 9 or 25 ° GH.
  • the wash powder was added in a dosage of 7.5 g/I. The differences in reflectance of the test clothes before and after the wash ( R * 460) were recorded.

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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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)

Claims (15)

1. Waschmittelzusammensetzung in Teilchenform, die als ein erstes fein verteiltes Material eine Fettsäuremischung, in der bis zu 35 Mol% ungesättigten Fettsäuren vorliegen können, wobei die Mischung bis zu einem Grad von 25-60 Mol% neutralisiert worden ist, und als ein zweites fein verteiltes Material eine Base in einer Menge enthält, die ausreicht, den pH der Zusammensetzung bei einer Konzentration von 0.5 Gew.-% in Wasser von höher als 8 zu liefern.
2. Waschmittelzusammensetzung in Pulverform nach Anspruch 1, die 30-80% der teilweise neutralisierten Fettmischung enthält.
3. Waschmittelzusammensetzung in Teilchenform nach Anspruch 1 oder Anspruch 2, wobei die Mischung der Fettsäuren im wesentlichen aus 5-20 Mol% C16-C18 ungesättigten Fettsäuren, und 95-80 Mol% einer Mischung von C8-C14 gesättigter Fettsäuren und C16-C18 gesättigter Fettsäuren in einem Verhältnis von 3:1-1:2 besteht.
4. Waschmittelzusammensetzung in Teilchenform nach einem der vorhergehenden Ansprüche, wobei die Base Natriumkarbonat oder alkalisches Natriumsilikat ist.
5. Waschmittelzusammensetzung in Teilchenform nach einem vorhergehenden Anspruch, die zusätzlich ein seifenfreies waschaktives Material umfaßt.
6. Waschmittelzusammensetzung in Pulverform nach Anspruch 5, die bis zu 10 Gew.-% anionisches und/oder nichtionisches Detergenzmaterial im ersten granulären Material enthält.
7. Waschmittelzusammensetzung in Pulverform nach Anspruch 5, die zusätzlich ein flüssiges nichtionisches Material auf einem porösen anorganischen Träger umfaßt.
8. Waschmittelzusammensetzung in Teilchenform nach einem vorhergehenden Anspruch, die zusätzlich ein Peroxibleichmittel-System und/oder alkalisches Natriumsilikat und/oder eine Anti-Schaum-Verbindung und/oder ein Enzym umfaßt.
9. Fettsäureseifenmaterial in Teilchenform, das als ein Ausgangspulver zur Herstellung von Waschmitttelpulvern geeignet ist, das im wesentlichen aus einer Fettsäuremischung, in der bis zu 35 Mol% ungesättigte Fettsäuren vorliegen können, wobei die Mischung bis zu einem Grad von 25-60 Mol% neutralisiert worden ist, besteht.
10. Fettsäureseifenmaterial in Teilchenform nach Anspruch 9, wobei die Mischung von Fettsäuren im wesentlichen aus 5-20 Mol% C16-C18 ungesättigten Fettsäuren und 95-80 Mol% einer Mischung von C8-C14 gesättigten Fettsäuren und C16-C18 gesättigten Fettsäuren in einem Verhältnis von 3:1-1:2 besteht.
11. Fettsäurenseifenzusammensetzung in Teilchenform nach Anspruch 9 oder 10 in der Form von Prillgranalien oder Strängen.
12. Fettsäurenseifenmaterial in Teilchenform nach einem der Ansprüche 9 bis 11, bei dem der Grad der Neutralisation 30-40 Mol% beträgt.
13. Verfahren zur Herstellung des Fettsäureseifenmaterials in Teilchenform nach Anspruch 9, gekennzeichnet durch die Schritte des Schmelzen einer Mischung von Fettsäuren, die gegebenenfalls ein oder mehrere Seifen enthält, teilweises Neutralisieren der Mischung, falls notwendig durch Zufügung einer Base, und Umwandlung dieser in eine feste Teilchenform.
14. Verfahren nach Anspruch 13, dadurch gekennzeichnet, daß das Fettsäurenseifenmaterial in Teilchenform durch Sprühkühlen der teilweise neutralisierten geschmolzenen Mischung von Fettsäuren zur Bildung von Prillgranalien hergestellt wird.
15. Verfahren nach Anspruch 13 oder 14, dadurch gekennzeichnet, daß die Mischung von Fettsäuren durch Zugabe von Natriumcarbonat und/oder alkalischem Natriumsilikat teilweise neutralisiert wird.
EP19890200221 1988-02-12 1989-02-02 Waschmittelzusammensetzung in Teilchenform Expired - Lifetime EP0328190B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB888803263A GB8803263D0 (en) 1988-02-12 1988-02-12 Particulate laundry detergent composition
GB8803263 1988-02-12

Publications (3)

Publication Number Publication Date
EP0328190A2 EP0328190A2 (de) 1989-08-16
EP0328190A3 EP0328190A3 (en) 1990-10-24
EP0328190B1 true EP0328190B1 (de) 1994-05-04

Family

ID=10631597

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19890200221 Expired - Lifetime EP0328190B1 (de) 1988-02-12 1989-02-02 Waschmittelzusammensetzung in Teilchenform

Country Status (5)

Country Link
EP (1) EP0328190B1 (de)
JP (1) JPH0668120B2 (de)
DE (1) DE68915015T2 (de)
ES (1) ES2051983T3 (de)
GB (1) GB8803263D0 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020222996A1 (en) * 2019-04-29 2020-11-05 The Procter & Gamble Company A process for making a laundry detergent composition
RU2773345C1 (ru) * 2019-04-29 2022-06-02 Дзе Проктер Энд Гэмбл Компани Способ получения композиции моющего средства для стирки

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5002377A (en) * 1988-07-07 1991-03-26 City Of Hope Multi-specimen slides for immunohistologic procedures
GB9618877D0 (en) * 1996-09-10 1996-10-23 Unilever Plc Process for preparing high bulk density detergent compositions
JP2011246682A (ja) * 2010-05-24 2011-12-08 Touki Corp 粉末洗濯用洗剤
CA2855467A1 (en) * 2013-07-02 2015-01-02 Milk Specialties Global Partial neutralization of free fatty acid mixtures with potassium, livestock feed compositions including them, and methods of making same

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB989007A (en) * 1961-01-23 1965-04-14 Procter & Gamble Detergent bar
BE755190A (fr) * 1969-08-25 1971-02-24 Procter & Gamble Compositions de savon de toilette
JPS5230962B2 (de) * 1972-12-12 1977-08-11
JPS5231202B2 (de) * 1973-11-01 1977-08-13
JPS5487707A (en) * 1977-12-26 1979-07-12 Kao Corp Soap for scouring pads
EP0042647A1 (de) * 1980-06-20 1981-12-30 Unilever N.V. Teilchenförmige, Seife enthaltende Reinigungsmittelzusammensetzung
ES2020729A6 (es) * 1990-08-01 1991-09-01 Asturiana De Zinc Sa Instalacion para desprender la capa de zinc depositada por electrolisis sobre catodos planos y catodo utilizado.

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020222996A1 (en) * 2019-04-29 2020-11-05 The Procter & Gamble Company A process for making a laundry detergent composition
CN113728083A (zh) * 2019-04-29 2021-11-30 宝洁公司 用于制备衣物洗涤剂组合物的方法
RU2773345C1 (ru) * 2019-04-29 2022-06-02 Дзе Проктер Энд Гэмбл Компани Способ получения композиции моющего средства для стирки

Also Published As

Publication number Publication date
ES2051983T3 (es) 1994-07-01
DE68915015T2 (de) 1994-08-18
EP0328190A3 (en) 1990-10-24
JPH01268799A (ja) 1989-10-26
EP0328190A2 (de) 1989-08-16
DE68915015D1 (de) 1994-06-09
GB8803263D0 (en) 1988-03-09
JPH0668120B2 (ja) 1994-08-31

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