EP0924291B2 - Wässrige Weichspülmittel mit verbessertem Weichgriff - Google Patents

Wässrige Weichspülmittel mit verbessertem Weichgriff Download PDF

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Publication number
EP0924291B2
EP0924291B2 EP98119569A EP98119569A EP0924291B2 EP 0924291 B2 EP0924291 B2 EP 0924291B2 EP 98119569 A EP98119569 A EP 98119569A EP 98119569 A EP98119569 A EP 98119569A EP 0924291 B2 EP0924291 B2 EP 0924291B2
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EP
European Patent Office
Prior art keywords
component
fatty acid
test
fabric
water
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
EP98119569A
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German (de)
English (en)
French (fr)
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EP0924291A1 (de
EP0924291B1 (de
Inventor
Axel Euler
Michael Fender
Hans-Jürgen Dr. Köhle
Hans-Georg Schiesser
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.)
Evonik Goldschmidt Rewo GmbH
Original Assignee
Goldschmidt Rewo GmbH
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Publication of EP0924291A1 publication Critical patent/EP0924291A1/de
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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
    • C11D1/38Cationic compounds
    • C11D1/62Quaternary ammonium 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
    • C11D3/0005Other compounding ingredients characterised by their effect
    • C11D3/001Softening compositions
    • C11D3/0015Softening compositions liquid

Definitions

  • the present invention relates to fabric softeners in the form of aqueous emulsions or dispersions.
  • cationic compounds are used as fabric softeners, for example quaternary ammonium compounds which, in addition to long-chain alkyl radicals, may also contain ester or amide groups, for example as described in US Pat. Nos. 3,449,033, 3,644,203, 3,946,115, 3,997,453 and 4,073,735, 4119 545. These components are added to the rinse bath alone or in mixtures with other cationic or even neutral substances in the form of aqueous dispersions.
  • ammonium compounds containing ester bonds as described, for example, in EP-A-0 239 910, US Pat. No. 3,915,867, US Pat. No. 4,137,180, US Pat. No. 4,830,771.
  • WO-A-94/20597 relates to concentrated softeners containing quaternary ammonium compounds in which the long-chain fatty acid residues contain 11 to 21 carbon atoms and have iodine numbers in the range of 5 to 100.
  • US-A-5,637,743 discloses the provision of a fabric softener containing quaternary ammonium salts wherein the fatty acid moieties contain 5 to 23 carbon atoms, the ratio of fatty acid: amine is 1.85 to 1.40 and iodine numbers are in the range of 10 to 33.
  • ester compounds based on triethanolamine such as N-methyl-N, N-bis (beta-C 14-18 -acyloxyethyl), N-beta-hydroxyethyl ammonium methosulfate, which are sold under trade names such as TETRANYL® AT 75 (trademark of KAO Corp.), STEPANTEX® VRH 90 (trademark of Stepan Corp.) or REWOQUAT® WE 18 (trademark of Witco Surfactants GmbH).
  • Reverse wetting is generally understood to mean the absorption of moisture by the fiber.
  • a defective reverse wetting effect has a disadvantageous effect where larger amounts of moisture are to be absorbed by the skin surface.
  • the object of the invention was to overcome the abovementioned disadvantages of conventional fabric softener formulations and to provide fabric softeners which, in addition to good biodegradability, have a substantially improved level of good soft feel while retaining a good repellency.
  • the object has been achieved by using quaternary fatty acid aminal alcohol esters of triethanolamine with partially hydrogenated fatty acids in a ratio of 1: 1.6 to 1: 2 in alcohols or glycols.
  • the quaternary compounds of the general formula I used in accordance with the invention are prepared by esterification of triethanolamine with fatty acid and subsequent quaternization by processes which are generally known in the art.
  • the fat components used for the esterification or transesterification are the monobasic fatty acids known and customary in this field and based on natural vegetable and animal oils with in particular 14-18 carbon atoms, such as tallow fatty acids and palm oil fatty acids or their methyl or ethyl esters.
  • the content of these fatty acids or fatty acid esters of unsaturated constituents is adjusted by the known catalytic hydrogenation to iodine numbers between 15-25, or by mixing fully hydrogenated with non-hydrogenated fat components.
  • the iodine number is the amount of iodine absorbed by 100 g of the compound to saturate the double bonds.
  • Partially hydrogenated tallow fatty acids and palm oil fatty acids with iodine numbers between 15-25 are preferred according to the invention. They are commercial products and are offered by various companies under their respective trade names.
  • the esterification or transesterification is carried out by known methods.
  • the triethanolamine with the desired degree of esterification corresponding amount of fatty acid or fatty acid ester optionally in the presence of a catalyst, for.
  • methanesulfonic acid reacted under nitrogen at 160-240 ° C and distilling off the water of reaction or the alcohol forming continuously, to optionally complete the reaction, the pressure can be reduced.
  • the subsequent quaternization is carried out by known methods.
  • the procedure is preferably such that the ester, optionally with the concomitant use of a solvent, preferably with isopropanol, ethanol, 1,2-propylene glycol and / or dipropylene glycol, at 60-90 ° C with equimolar amounts of the quaternizing agent with stirring, optionally under pressure and the completion of the reaction is monitored by controlling the total amine number.
  • Examples of the quaternizing agents used are short-chain dialkyl phosphates and sulfates, such as diethyl sulfate, dimethyl phosphate, diethyl phosphate, short-chain halogenated hydrocarbons; In particular, according to the invention dimethyl sulfate is used.
  • TAA triethanolamine
  • fatty acids were reacted and quaternized by the usual methods.
  • Fatty acid I Tallow fatty acid having an acid number of 200-210, an iodine value of 15-25 and a C chain distribution of ⁇ C - 16 about 2% C - 16 about 26% C - 16 ' about 2% C - 17 about 3% C - 18 about 48% C - 18 ' about 15% C - 18 " ⁇ 1%
  • Fatty acid III Tallow fatty acid having an acid number of 200-210, an iodine value of 45-55 and a C chain distribution of ⁇ C - 16 about 4% C - 16 about 26% C - 16 ' about 2%
  • TEA fatty acid I 1: 2
  • Component B TEA: fatty acid I 1: 1.6
  • Component C TEA: fatty acid II 1: 2
  • Component D TEA: fatty acid II 1: 1.6
  • Component E TEA: fatty acid III 1: 2
  • Component F TEA: fatty acid III 1: 1.6
  • the fabric softeners are prepared by emulsifying or dispersing the respective individual components in water. In this case, the usual procedures in this field can be used.
  • the usual procedure is to initially charge the water preheated to about 10 ° C. below the clear melting point of the plasticizer, then, with good stirring, first the dye solution, then the optionally required antifoam emulsion and finally the clear melt of the individual plasticizers. After adding a partial amount of an electrolyte solution, perfume oil is added, followed by the remaining amount of electrolyte solution, and then allowed to cool to room temperature while stirring.
  • the fabric softeners according to the invention may contain the specified components within the usual limits in this field, such as 15-22 wt .-% of the compounds of general formula (I); 2-5 wt .-% of a solvent such as in particular isopropanol, ethanol, propylene glycol, dipropylene glycol; 0.5-1.5% by weight of an alkali and / or alkaline earth salt; 0.5-1.5% by weight of perfume oil and the remainder to 100% by weight (ad 100) of water.
  • a solvent such as in particular isopropanol, ethanol, propylene glycol, dipropylene glycol
  • 0.5-1.5% by weight of an alkali and / or alkaline earth salt 0.5-1.5% by weight of perfume oil and the remainder to 100% by weight (ad 100) of water.
  • the fabric softeners according to the invention are added following the actual washing process in the last rinse.
  • Application dilution after dilution with water ranges from 0.1 to 10 g of fabric softener per liter of treatment liquor, depending on the application.
  • test fabric (about 3 kg cotton twill fabric, 100% cotton, supplier: WFK-Testgewebe GmbH, Krefeld) is washed twice with 100 g test detergent and then without detergent (each 95 ° C program with prewash) , The test fabric is hung for one day at room temperature to dry. After drying, test strips of about 25 cm in length and 1.5 cm in width are cut. It is important to ensure that all test strips of a test series have the same thread course.
  • test strips are marked with a ballpoint pen. Holes are punched at both ends of the test strips; while a 5 cm thick fabric edge should be preserved.
  • the corresponding amount of demineralized water is introduced and stirred in 0.025%, based on the solids content, of the product to be tested.
  • a blank test is carried out by submitting demineralized water in the immersion bath.
  • test strips are added, stirred for 5 minutes at about 50 rpm using a magnetic stirrer and then left for 5 minutes without stirring. Subsequently, the test strips are dried hanging at room temperature for 24 h. After this time, draw a line parallel to the long outer edges with a water-soluble felt pen on the smooth side of each strip.
  • test strips blank + test product (s)
  • the immersion device with the strips is placed in the tub filled with demineralized water (about 10 l) to a height of 8 cm and left there for 5 min. 10 min after removing the immersion device from the tub, the height of rise of the water, the It is important to make sure that the lower edge of the hole, with its upper side, rests directly against the (hanging) hook in order to avoid reading errors.
  • the demineralized water must be renewed after each attempt.
  • test fabric fabric "Duosoft", 100% cotton, supplier: Vossen
  • test fabric 100% cotton, supplier: Vossen
  • a fixed mesh size of 15 results in a liquor ratio of 1: 5. After washing, the test fabric is hung for one day at room temperature to dry and then stored until processing at room temperature.
  • the calculated amounts of fabric softener are placed in the beakers at 15-20 ° C and filled with tap water of about 9 ° dH and 15-20 ° C to 2 l. The mixture is then stirred on the magnetic stirrer until homogeneous dispersions or solutions have been present.
  • a blank test is carried out by pure tap water is presented in the dip. 1 piece of test fabric is dipped per rinse bath. After 10 minutes, the tissue is removed from the rinse bath, gently wrung out, gently shaken three times and dried for one hour at room temperature in a single-layered suspension.
  • test fabric thus treated is cut into 10 equal pieces (about 16x25 cm). Each subject receives a new test piece for the assessment. It must be prevented that the test pieces are "softened” after some attempts to grip.
  • test fabrics treated with different softeners are now compared in pairs.
  • the contestants can distribute whole points between 0 and 5, where 0 point means bad (hard) and 5 points means good (soft).
  • dispersions are prepared from the components mentioned:

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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)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
EP98119569A 1997-12-18 1998-10-16 Wässrige Weichspülmittel mit verbessertem Weichgriff Expired - Lifetime EP0924291B2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19756434 1997-12-18
DE19756434A DE19756434A1 (de) 1997-12-18 1997-12-18 Wäßrige Weichspülmittel mit verbessertem Weichgriff

Publications (3)

Publication Number Publication Date
EP0924291A1 EP0924291A1 (de) 1999-06-23
EP0924291B1 EP0924291B1 (de) 2003-09-03
EP0924291B2 true EP0924291B2 (de) 2006-07-26

Family

ID=7852465

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98119569A Expired - Lifetime EP0924291B2 (de) 1997-12-18 1998-10-16 Wässrige Weichspülmittel mit verbessertem Weichgriff

Country Status (6)

Country Link
US (1) US6110887A (pl)
EP (1) EP0924291B2 (pl)
CA (1) CA2254399C (pl)
DE (2) DE19756434A1 (pl)
ES (1) ES2206808T5 (pl)
PL (1) PL195045B1 (pl)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19855366A1 (de) * 1998-12-01 2000-06-08 Witco Surfactants Gmbh Niedrigkonzentrierte, hochviskose wäßrige Weichspülmittel
AU4856399A (en) * 1999-07-01 2001-01-22 Procter & Gamble Company, The Quaternary nitrogen compound, fabric care composition containing same, and process for forming same
US7371718B2 (en) * 2005-04-22 2008-05-13 The Dial Corporation Liquid fabric softener
WO2011149475A1 (en) 2010-05-28 2011-12-01 Colgate-Palmolive Company Fatty acid chain saturation in alkanol amine based esterquat
EP2997958B1 (de) 2014-09-22 2021-03-10 Evonik Operations GmbH Emulsion enthaltend flüssige esterquats und polymerverdicker
EP2997959B1 (de) 2014-09-22 2019-12-25 Evonik Operations GmbH Formulierung enthaltend esterquats basierend auf isopropanolamin und tetrahydroxypropylethylenediamin

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2021900A6 (es) * 1989-07-17 1991-11-16 Pulcra Sa Procedimiento de obtencion de tensioactivos cationicos derivados de amonio cuaternario con funcion amino-ester.
DE4101251A1 (de) * 1991-01-17 1992-07-23 Huels Chemische Werke Ag Fettsaeureester des n-methyl-n,n,n-trihydroxyethyl-ammonium-methyl- sulfat enthaltende waessrige emulsionen
ES2094893T3 (es) * 1991-12-31 1997-02-01 Stepan Europe Tensioactivos a base de compuestos de amonio cuaternario, procedimientos de preparacion, bases, y composiciones suavizantes derivadas.
PT687291E (pt) * 1993-03-01 2000-09-29 Procter & Gamble Composicoes concentradas e biodegradaveis amaciadoras de texteis a base de amonio quaternario e compostos contendo cadeias de acido gordo insaturado possuindo um valor de iodo intermedio
JP3235915B2 (ja) * 1993-07-13 2001-12-04 ファナック株式会社 ワイヤ結線状態表示装置
DE4339643C1 (de) * 1993-11-20 1995-06-08 Henkel Kgaa Verfahren zur Herstellung von festen Esterquats
DE4400927A1 (de) * 1994-01-14 1995-07-20 Henkel Kgaa Wäßrige Lösungen von quaternierten Fettsäuretriethanolaminester-Salze
DE4405702A1 (de) * 1994-02-23 1995-08-24 Witco Surfactants Gmbh Hochkonzentrierte wäßrige Weichspülmittel mit verbesserter Lagerstabilität
US5869716A (en) * 1994-03-18 1999-02-09 Henkel Kommanditgesellschaft Auf Aktien Process for the production of esterquats
US5503756A (en) * 1994-09-20 1996-04-02 The Procter & Gamble Company Dryer-activated fabric conditioning compositions containing unsaturated fatty acid
DE4446137A1 (de) * 1994-12-23 1996-06-27 Huels Chemische Werke Ag Quaternierte Triethanolamindifettsäureester
EP0850291B1 (en) * 1995-08-31 2002-01-30 Colgate-Palmolive Company Stable fabric softener compositions
EP0768369A1 (en) * 1995-10-11 1997-04-16 The Procter & Gamble Company Fabric softener compositions
US5916863A (en) * 1996-05-03 1999-06-29 Akzo Nobel Nv High di(alkyl fatty ester) quaternary ammonium compound from triethanol amine

Also Published As

Publication number Publication date
CA2254399A1 (en) 1999-06-18
EP0924291A1 (de) 1999-06-23
US6110887A (en) 2000-08-29
DE59809482D1 (de) 2003-10-09
ES2206808T3 (es) 2004-05-16
PL330381A1 (en) 1999-06-21
DE19756434A1 (de) 1999-06-24
ES2206808T5 (es) 2007-04-01
PL195045B1 (pl) 2007-08-31
EP0924291B1 (de) 2003-09-03
CA2254399C (en) 2007-07-10

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