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Title:
NON-PERMANENT SOFTENING FINISHING OF TEXTILE PIECE GOODS IN JET-DYEING MACHINES, AND COMPOSITIONS SUITABLE FOR THIS PURPOSE
Document Type and Number:
WIPO Patent Application WO/2001/077434
Kind Code:
A2
Abstract:
Aqueous dispersions (W) which comprise the following components: (A) at least one condensation product of at least one C¿12-24?-fatty acid or at least one low-molecular-weight alkyl ester thereof with 2-[($g(b)-hydroxyethyl)-amino]-ethylamine, (B) at least one (C¿12-24?-fatty acid)-[$g(g)-(N,N-dimethylamino)-propyl]amide, and (C) at least one low-molecular-weight carboxylic acid, and optionally (D) at least one oligoethylene glycol, liquid at ambient temperature, and/or (E) at least one formulation additive, and are substantially free from dispersion-modifying other additives (Z), in particular concentrated dispersions (W'), are eminently suitable as softener compositions for the non-permanent, softening finishing of dyed and/or optically brightened textile piece goods in rope form or tubular form by exhaust methods from aqueous liquors in jet dyeing machines.

Inventors:
DANNER BERNARD
Application Number:
PCT/IB2001/000589
Publication Date:
October 18, 2001
Filing Date:
April 10, 2001
Export Citation:
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Assignee:
CLARIANT INT LTD (CH)
CLARIANT FINANCE BVI LTD
International Classes:
C11D1/645; C11D1/72; C11D3/00; C11D3/20; C11D3/32; D06M13/17; D06M13/184; D06M13/188; D06M13/405; D06M13/419; D06M13/46; D06M15/53; D06M15/643; D06P1/00; D06P1/649; D06P1/653; D06P5/06; (IPC1-7): D06M13/00
Domestic Patent References:
WO1992018685A11992-10-29
Foreign References:
DE2841076B11979-06-13
DE3810108A11988-10-13
EP0188242A21986-07-23
DE3334575A11984-04-05
Attorney, Agent or Firm:
D'haemer, Jan (Clariant International Ltd. Rothausstrasse 61 Muttenz 1, CH)
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Claims:
CLAIMS
1. Use of aqueous dispersions (W) which comprise the following components: (A) at least one condensation product of at least one C ; 224fatty acid or at least one lowmolecular alkyl ester thereof with 2[(ßhydroxyethyl)amino] ethylamine, (B) at least one optionally protonated (Cl2 24fatty acid)[y(N, Ndimethylamino) propyl]amide and (C) at least one lowmolecular carboxylic acid and optionally (D) at least one oligoethylene glycol which is liquid at room temperature and/or (E) at least one formulation additive, and are essentially free from dispersionmodifying other additives (Z), as softener compositions for the nonpermanent, softening finishing of dyed and/or optically brightened textile piece goods in rope form or tubular form by exhaust methods from aqueous liquor in jetdyeing machines.
2. Use according to Claim 1, characterized in that the dispersionmodifying additives (Z) are waxes, fats or oils and their derivatives, epoxides, alkyl or hydroxyalkyl esters, saccharides and saccharide derivatives, polyorganosiloxanes or polymers of ethylenically unsaturated monomers, and component (E) is (EI) at least one agent for protection against the damaging action of micro organisms and/or (E2) at least one defoamer.
3. Use according to Claim 1 or 2, characterized in that in (W) the weight ratio (B)/ (A) is in the range from 6/100 to 60/100, the weight ratio (D)/ (A) is in the range from 0 to 300/100 the weight ratio (E)/ (A) is in the range from 0 to 6/100 the content of (A) is in the range from 4 to 50 % by weight, the content of (C) is at least 0.5 equivalents of (C) per equivalent of the total of basic amino groups in (A) + (B), the dry substance content is in the range from 8 to 60 % by weight, and the viscosity is < 1000 4.
4. Use according to one of Claims 1 to 3, characterized in that (A) is an openchain condensation product which consists principally of the compounds of the formulae RCONHCHzCH2NHCH2CH2OH (I), RCONHCH2CH2N (COR)CH2CH2OH (II), RCONHCH2CH2NHCH2CH20COR(ici) and/or RCONHCH2CH2N (COR)CH2CH20COR (IV) in which RCOdenotes the radical of a Cl2 24fatty acid.
5. Use according to one of Claims I to 4 for the nonpermanent, softening finishing of dyed and/or optically brightened, textile piece goods made from natural, optionally modified fibrous material and/or from semisynthetic fibrous material, optionally as a blend with fully synthetic fibrous material.
6. Use according to one of Claims 1 to 5, wherein (W) is an aqueous dispersion essentially consisting of (A), (B), (C) and water and optionally at least one of additives (D) and/or (E).
7. Aqueous (Z)free composition (W) which is an aqueous dispersion (W') essentially consisting of (A), (B), (C) and water and optionally at least one of additives (D) and/or (E), as defined in one of Claims 3 to 6, which has a content of (A) in the range from 4 to 50 % by weight and a dry substance content in the range from 8 to 60 % by weight, and whose viscosity at room temperature is < 1000 cP, and in which the weight ratio (B)/ (A) is in the range from 6/100 to 60/100, the weight ratio (D)/ (A) is in the range from 0 to 300/100 the weight ratio (E)/ (A) is in the range from 0 to 6/100 and the content of (C) is at least 0.5 equivalents of (C) per equivalent of the total of basic amino groups in (A) + (B).
8. Aqueous dispersion (W') according to Claim 7, with a pH in the range from 3 to 8.
9. Process for the production of the aqueous dispersions (W') according to Claim 7 or 8, characterized in that a mixture of (A) and (B) in the respective necessary amount ratio is mixed with water and with (C), and optionally at least one of components (D) and (E) in the respective necessary amount ratio is admixed.
Description:
NON-PERMANENT SOFTENING FINISHING OF TEXTILE PIECE GOODS IN JET- DYEING MACHINES, AND COMPOSITIONS SUITABLE FOR THIS PURPOSE In the softening finishing-particularly also in non-permanent softening finishing-of textile piece goods in jet-dyeing machines, a major problem consists in that the treatment liquors in these machines are subjected to very strong dynamic stresses in which strong shear forces arise which can exert a destabilizing action on the respective treatment agent, so that this can have the consequence of a reduction in the action and/or an impairment of the treatment liquor and/or of the treated material. In treatment for softening finishing of dyed or optically brightened goods, in particular also in subsequent treatment in the same jet-dyeing machine in which the goods have been dyed or optically brightened, it is also important that the respective dyeing or optical brightening is not impaired by the treatment agent used and that the soft handle of the finished goods is significantly improved. The quality of the waste water resulting from the process is also important, and thus it is also desired that the softener builds up on the substrate as well as possible.

It has now been found that through the use of the compositions (W) defined below, the above- mentioned problems and difficulties can be substantially solved or overcome in a surprisingly simple manner and the requirements mentioned can be substantially satisfied and non-permanent softening finishes of high quality can be obtained.

The invention relates to the use of the defined compositions (W) for the non-permanent softening finishing of dyed and/or optically brightened piece goods in jet-dyeing machines, to certain concentrated dispersions of the (W) type, and to their production.

A first subject-matter of the invention is thus the use of aqueous dispersions (W) which comprise the following components: (A) at least one condensation product of at least one Cl2 24-fatty acid or at least one low- molecular alkyl ester thereof with 2-[(ß-hydroxyethyl)-amino]-ethylamine, (B) at least one (C. -fatty acid)- [y- (N, N-dimethylamino)-propyl]-amide and (C) at least one low-molecular-weight carboxylic acid and optionally (D) at least one oligoethylene glycol which is liquid at room temperature and/or (E) at least one formulation additive, and are essentially free from dispersion-modifying other additives (Z), as softener compositions for the non-permanent, softening finishing of dyed and/or optically brightened textile piece goods in rope form or tubular form by exhaust methods from aqueous liquor in jet-dyeing machines.

Condensation products of type (A) are known or can be produced in a manner known per se, particularly by acylation of 2-[(ß-hydroxyethyl)-amino]-ethylamine with a C12-24-fatty acid with elimination of water, or also with a low-molecular alkyl ester thereof with elimination of the cor- responding low-molecular alcohol. The molar ratios of the fatty acids or alkyl esters thereof to the 2- [ (P-hydroxyethyl)-amino]-ethylamine are advantageously selected in such a way that the condensation product contains diacylated products; this molar ratio is advantageously > 1.1/1 and < 2.5/1; it is preferably in the range from 1.2/1 to 2.2/1, particularly preferably from 1.4/1 to 2/1.

Suitable fatty acids are any desired, preferably linear fatty acids having 12 to 24, advantageously 14 to 22, carbon atoms, which are conventional per se, preferably saturated fatty acids, for example lauric acid, myristic acid, palmitic acid, stearic acid, arachic acid and behenic acid. Both individual acids and also technical-grade acids (acid mixtures) can be employed, such as, for example, hydrogenated tallow fatty acid, hydrogenated technical-grade oleic acid or hydrogenated technical-grade soya oil acid. Of the said acids, those having 14 to 18 carbon atoms, and also technical-grade mixtures of such acids, are preferred. Low-molecular alkyl esters which come into consideration are, for example, those in which the ester-forming alkyl radical contains 1 to 4 carbon atoms (for example methyl, ethyl, isopropyl or n-butyl), principally Cl 2-alkyl, particularly methyl. Of the fatty acid alkyl esters and the fatty acids, the fatty acids are preferred.

The condensation advantageously takes place in anhydrous medium, most simply in the absence of solvents, for example at temperatures in the range from 140 to 200°C, preferably from 170 to 190°C, advantageously under an inert atmosphere (for example under nitrogen) and/or advan- tageously under reduced pressure.

The acylation can take place on the primary amino group, on the secondary amino group and/or also on the hydroxyl group, and, depending on the molar ratio, monoacylated, diacylated and/or triacylated products may be formed, the acylation principally being an amidation, and essentially no cyclic products being formed. The acylation products are essentially open-chain products. In particular, (A) may comprise monoamides, diamides, ester monoamides and ester diamides of N- (P-hydroxyethyl)-ethylenediamine with the said fatty acids, principally compounds of the formula R-CO-NH-CH2-CH2-NH-CH2-CH2-OH R-CO-NH-CH2-CH2-N (CO-R)-CH2-CH2-OH (II), R-CO-NH-CH2-CH2-NH-CH2-CH2-O-CO-R (III) and/or R-CO-NH-CH2-CH2-N (CO-R)-CH2-CH2-0-CO-R (IV), in which R-CO-denotes the radical of a C) 2-24-fatty acid.

The condensation products (A) essentially consist of one or more of the products of the formulae (I), (II), (III) and (IV); (A) is preferably a mixture of these compounds, of which those of the formulae (I), (II) and (III) preponderate.

The (Cl2 24-fatty acid)-[y-(N, N-dimethylamino) propyl] amides which are suitable as component (B), in particular of the formula (H3C)2N-CH2-CH2-CH2-NH-CO-R (V), are known and/or can be produced by methods known per se, principally by acylation of y- (N, N-dimethylamino)-propylamine with fatty acids or low-molecular alkyl esters thereof, analogously to that described above for (A). The acylation is advantageously begun under

relatively mild temperature conditions, in particular below the boiling point of y- (N, N-dimethyl- amino)-propylamine, advantageously in the range from 100 to 130°C, and can then be continued at higher temperature, preferably from 130 to 190°C, and completed, preferably at from 150 to 190°C. Also this amidation can optionally be carried out under an inert atmosphere and/or under reduced pressure and preferably in the absence of solvents.

The two products (A) and (B) produced in this way can be combined with one another, i. e. mixed, in the melt, and the mixture can then be cooled, for example with simultaneous formation of a free-flowing dry form, for example granules, pellets or tablets.

According to a particular feature of the invention, the two acylations, i. e. that of 2- [ (P-hydroxy- ethyl)-amino]-ethylamine and that of y- (N, N-dimethylamino)-propylamine, can be carried out in a single working step by, for example, mixing the two amines with one another and then carrying out the acylation with the total amount of the respective fatty acid or of the respective fatty acid alkyl ester at rising temperature in such a way that the acylation is begun at milder temperatures, in particular < 130°C, and is then completed on increasing the temperature, or by initially intro- ducing the fatty acid or the respective fatty acid alkyl ester and then firstly adding the y- (N, N-di- methylamino)-propylamine at temperatures of < 130°C and then adding the 2- [ (P-hydroxy- ethyl)-amino]-ethylamine at higher temperature, preferably 130-150°C, and completing the acylation on a further increase in the temperature, preferably at from 150 to 190°C. The mixture can then, as mentioned above, preferably be cooled with simultaneous formation of a pourable particulate dry form, for example granules, pellets or tablets.

The (B)/ (A) weight ratio is advantageously in the range from 6/100 to 60/100, preferably from 10/100 to 40/100, particularly preferably from 13/100 to 30/100.

The compositions (W) can be produced in a simple manner, in particular by mixing a mixture of (A) and (B) with water and with (C), and optionally admixing at least one of components (D) and (E).

Suitable as (C) are, in particular, aliphatic monocarboxylic acids, advantageously saturated, principally those having 1 to 3 carbon atoms, preferably formic acid, acetic acid, propionic acid and lactic acid, of which acetic acid is particularly preferred.

Component (B), particularly also as corresponds to the formula (V), contains a tertiary proton- atable amino group. Component (A) may, depending on the degree of acylation, have a different content of basic, protonatable amino groups, principally as corresponds to the compounds of the formulae (I) and (III). The content of protonatable amino groups can be assessed by determining the amine number. The amine number of (A) is, for example, in the range from 30 to 100, prefer- ably from 50 to 80, particularly preferably from 55 to 70 mg of KOH per g of condensate (A).

The content of (C) is advantageously at least 0.5 equivalents of (C) per equivalent of the total of the basic amino groups in (A) + (B). The mixture of (A) + (B) is preferably protonated to exhaustion, i. e. preferably 21 equivalent of (C) are employed per equivalent of basic amino groups in (A) + (B). Preferably, from 0.5 to 6 mole-equivalents of (C) are employed per mole- equivalent of basic amino groups in (A) + (B), particularly preferably from 1 to 5, above all from 1. 5 to 4 mole-equivalents of (C) per mole-equivalent of basic amino groups in (A) + (B).

The acid (C) is advantageously employed in the form of an aqueous solution, for example as a solution of the determined amount of (C) in the entire amount of water necessary for the produc- tion of (W) or also only in part thereof, where in the latter case the precise desired concentration can be adjusted with further water. The mixing of condensate (A) and amide (B) with water and acid (C) advantageously takes place through addition of the pourable form of the mixture of (A) + (B) to the aqueous solution of the acid (C) at elevated temperature, for example in the range from 30 to 85°C, preferably from 50 to 75°C.

Suitable as (D) are in general oligoethylene glycols which are liquid at room temperature (= 20°C), in particular those which have an average molecular weight Mw in the range from 150 to 400, preferably from 200 to 400 (for example polyethylene glycol 200,300 or 400), and which are preferably substantially free from mono-and diethylene glycols. Component (D) may be present if desired. The (D)/ (A) weight ratio can, for example, be in the range from 0 to 300/100.

It is advantageous in accordance with the invention, that a certain proportion of (D) is present in (W); the (D)/ (A) weight ratio is preferably in the range from 20/100 to 260/100, particularly preferably in the range from 35/100 to 140/100.

The aqueous dispersions (W) to be employed according to the invention are essentially free from the dispersion-modifying additives (Z). By dispersion-modifying additives (Z) are meant those types and/or amounts of other products which significantly modify the appearance, the physical

form and/or the stability of the composition or also its action (in particular worsen the action and/or impair, for example, the viscosity, the flow properties, the storage stability, etc.).

As (Z) are principally meant high-molecular and/or water-insoluble products and/or compounds with three or more hydroxyl groups, as can otherwise occur in textile treatment compositions, but which in the compositions of the invention have an adverse effect on the production, on the stability and/or on the action. As (Z) are meant above all disturbing amounts of waxes, fats or oils and/or derivatives thereof, of epoxides, of alkyl or hydroxyalkyl esters, of saccharides and saccharide derivatives, of polyorganosiloxanes or of polymers of ethylenically unsaturated mono- mers, in particular in concentrations of > 1 % by weight, based on (W), particularly preferably also only > 0.5 % by weight, based on (W).

Optionally (W) may also comprise one or more formulation additives (E) which essentially serve to maintain the physical form of the dispersion (W).

These formulation additives are principally (El) at least one agent for protection against the damaging action of microorganisms, and/or (E2) at least one defoamer.

Suitable as (Ei) are in general usual commercial products as are in general commercially available as agents for inhibiting the growth of damaging microorganisms (for example fungi or bacteria) or biocides (for example fungicides or bactericides), and can also be employed in the low concentrations usually recommended, for example in concentrations of < 0.5 % by weight, preferably < 0.1 % by weight, in particular < 0.02 % by weight, based on the dispersion (W).

As (E2), it is generally possible to use any desired defoamers, as are known in general for aqueous systems, or are commercially available, for example polysiloxanes, oils, hydrophobic silicic acid or bisamides of ethylenediamine with higher saturated fatty acids (for example Cl630, in particular Cl8 24), principally ethylene bisstearamide. During transport or during handling of defoamer-free dispersions (W) or also on use thereof, foam may form temporarily, and the addition of (E2) serves essentially to accelerate or support the regression of the foam formed temporarily. (E2) can correspondingly be employed in very small amounts, for example in concentrations of < 1 % by weight, preferably < 0.5 % by weight, in particular < 0.2 % by weight, based on (W). If (E2) is a compound or also a mixture of compounds of the type of the products mentioned above under (Z), the concentration of this product is so small that it does not exert an

adverse effect on the physical form of the dispersion (W), i. e. (E2) is not a"dispersion- modifying"other additive in the sense of (Z).

The (E)/ (A) weight ratio is, for example, in the range from 0 to 6/100, advantageously below 4/100, preferably in the range from 0.01/100 to 2/100, particularly preferably from 0.05/100 to 1/100.

The (El)/(A) weight ratio is, for example, in the range from 0 to 1/100, advantageously below 0.5/100, preferably in the range from 0.001/100 to 0.2/100, particularly preferably from 0.002/100 to 0.1/100.

The (E2)/ (A) weight ratio is, for example, in the range from 0 to 5/100, advantageously below 3/100, preferably in the range from 0.01/100 to 1.8/100, particularly preferably from 0.045/100 to 0.9/100.

The additives (D) and/or (E) may be added when the other components (A), (B) and (C) and at least a part of the water have already been mixed with one another. Components (E) are advan- tageously added in the form of aqueous compositions (as are usually commercially available per se). If necessary, further water may also be added at the end for more precise adjustment of the concentration.

The dispersions (W) are principally those which essentially consist of (A), (B), (C) and water and optionally (D) and/or (E).

The dispersions (W) are advantageously produced in the form of concentrated dispersions (W'), in particular dispersions having a dry substance content in the range from 8 to 60 % by weight, preferably from 9 to 40 % by weight, particularly preferably from 10 to 30 % by weight, and in which the content of (A) is advantageously in the range from 4 to 50 % by weight, preferably from 6 to 30 % by weight, particularly preferably from 7 to 20 % by weight; the weight ratios of the respective components (B), (D) and (E) to component (A), and the molar ratio of component (C) to the total of components (A) + (B) are advantageously in the ranges indicated in detail above.

The compositions (W), and in particular (W'), are advantageously acidic to weakly basic. The pH of the concentrated compositions (W') is advantageously in the range from 3 to 8, preferably from 3.5 to 7, particularly preferably from 4 to 6.

These compositions (W) and (W') are in general liquid, in particular of fluid, and their viscosity at room temperature is advantageously < 1000 cP, preferably < 500 cP, in particular-above all for (W')-in the range from 30 to 500 cP, particularly preferably in the range from 40 to 200 cP.

A particular subject-matter of the invention is represented by these concentrated, (Z)-free disper- sions (W'), which have a content of (A) in the range from 4 to 50 % by weight, a dry substance content in the range from 8 to 60 % by weight, and whose viscosity at room temperature is < 1000 cP, and the weight ratios of the respective components (B), (D) and (E) to component (A), and the molar ratio of component (C) to the total of components (A) + (B) are in the ranges indicated in detail above. In particular, in (W') the weight ratio (B)/ (A) is in the range from 6/100 to 60/100, the weight ratio (D)/ (A) is in the range from 0 to 300/100 and the weight ratio (E)/ (A) is in the range from 0 to 6/100, and the content of (C) is at least 0.5 equivalents of (C) per equivalent of the total of basic amino groups in (A) + (B).

The preferred and particularly preferred amount ratios (B)/ (A), (D)/ (A) and (E)/ (A) in (W') and the preferred and particularly preferred contents of (A), contents of (C) and pH values, dry substance contents and viscosities are as indicated above for (W).

In particular, a subject-matter of the invention is also the concentrated dispersions (W') which essentially consist of (A), (B), (C) and water and optionally (D) and/or (E), in the stated concen- trations and quantitative ratios.

The concentrated dispersions (W') can be produced as described above. In particular, the process for the production of these concentrated aqueous softener compositions (W') is characterized in that a mixture of (A) and (B) in the respective necessary quantitative ratio is mixed with water and with (C), and optionally at least one of components (D) and (E) is admixed in the respective necessary quantitative ratio.

The dispersions (W) and in particular (W') are very storage-and temperature-stable and also stable to the action of high shear forces and are highly suitable for the finishing of textile sub- strates in jet-dyeing machines. They are liquid to highly fluid and can therefore also be metered very well. They serve as softeners for the non-permanent, softening finishing of dyed and/or optically brightened textile piece goods in jet-dyeing machines. The textile piece goods may be in any desired form as is suitable for treatment in jet-dyeing machines, in particular in rope form or tubular form, principally as woven or knitted fabrics, and can consist of any desired fibrous materials as are usual as textile fibres, in particular of natural, optionally modified fibrous material or semisynthetic and/or fully synthetic fibrous material. As natural, optionally modified or semisynthetic fibrous material, mention may be made, in particular, of optionally modified cellulose fibres (for example cotton, hemp, linen and mercerized cotton), regenerated cellulose (viscose or lyocel), cellulose acetate and natural, optionally modified polyamides (for example wool and Hercoset wool). As synthetic fibres, mention may be made of, for example: polyesters, polyamides, polyurethanes and acrylic polymers. Principally suitable for the process of the invention are substrates made from natural fibres and/or from modified or semisynthetic fibres, and their blends with synthetic fibres (for example as fibre blends or as a blended woven or knitted fabric, for example cotton/polyester, cotton/polyester/elastane or wool/polyamide).

The substrates are dyed or optically brightened. The respective dyes or optical brighteners used for this purpose can be any dyes or optical brighteners which are usually suitable per se for the respective substrate, for example direct dyes, reactive dyes, acid dyes, basic dyes, sulphur dyes, vat dyes and, especiallyly for synthetic fibres, also disperse dyes. As optical brighteners, suitable ones in each case can be used, in particular anionic or cationic brighteners or disperse brighteners, depending on the substrate.

The substrates may have been dyed or optically brightened by any desired conventional processes. In a preferred procedure, the substrates are dyed or optically brightened in the same jet-dyeing machine in which the finishing with (W) then takes place. For the dyeing or optically brightening of the preferred natural and optionally modified substrates in jet-dyeing machines, the anionic dyes (principally direct dyes, reactive dyes and acid dyes) and the anionic optical brighteners are preferred.

The softening finishing with (W) according to the invention may be carried out directly after dyeing or optically brightening, advantageously after any washing or (for dyeings with reactive dyes) soaping as may be necessary, and rinsing, or, optionally (for example for optical

brightenings or for dyeings with direct or acid dyes), also only rinsing, and optionally after any fixation-which may optionally be necessary, depending on the dyeing.

Suitable for the treatment with (W) according to the invention are any desired conventional jet- dyeing machines and any desired conventional goods-to-liquor ratios, for example substrate/- liquor ratios in the range from 1: 5 to 1: 20, preferably from 1: 6 to 1 : 12. The pH of the liquor is advantageously-depending on the dyeing or optical brightening of the substrate-in the acidic to weakly basic range, for example in the pH range from 4 to 8.5, advantageously from 4.5 to 8, preferably from 5 to 8. The finishing can take place under mild temperature conditions, for example in the temperature range from room temperature to 70°C, advantageously from 25 to 60°C, preferably from 30 to 50°C. The aqueous composition (W) is advantageously employed in concentrations as are sufficient to obtain a corresponding softening finishing. Even relatively low concentrations of (A) + (B) + (C) are sufficient to obtain an effective softening finishing, for example, calculated as still unprotonated components (A) + (B), a total concentration of (A) + (B) in the range from 0.02 to 4 % by weight, preferably from 0.05 to 2 % by weight, particularly preferably from 0.1 to 1 % by weight, based on the dry substrate.

During the finishing, practically no disturbing friction or creasing takes place, and the process can be carried out without flaws. The treated goods can then be removed from the machine, optionally centrifuged, and dried.

The softener compositions have optimum affinity to the substrates, on the one hand in order to build up practically completely on the substrates during the treatment in the jet-dyeing machine, so that they are able to fully display their softening action after drying of the treated substrates, and on the other hand in order to be bound to the substrates in a sufficiently labile manner so that they act as non-permanent finish and can then be washed out of the substrate again at the suitable or desired point in time-advantageously after make-up of the finished piece goods into finished goods (for example into items of clothing or other articles of use).

The softening finishing obtained in this way with (W) has a non-permanent character. The soft handle of the goods finished in accordance with the invention is very pleasant and not slippery and is ideally suitable for subsequent confection of the goods.

In the following Examples, parts denote parts by weight and percentages denote percentages by weight; the temperatures are given in degrees Celsius. In the Application Examples, the dyes are

employed in commercially available form with an active substance content of about 25 %, and the stated concentrations are based on this form. C. I. stands for Colour Index, dH for German degrees of hardness.

The defoamers and biocides employed in the Examples are the following: "Silikon Antischaumemulsion SE 2" (from Wacker Chemie, Germany), which is a %, aqueous, non-ionogenic silicone emulsion with pH 3.5-5.0, and"Saniprot 9408" (from Sanitized, Switzerland), which is a 1.5 %, aqueous solution of the hydrochloride of chlorinated 2-methyl-4-isothiazolin-3-one.

Example 1 1.1 Production of condensate (A 435 parts of stearic acid, technical grade (acid number 207.5) (mixture of stearic acid and palmitic acid) are heated to 180°C under nitrogen. 98 parts of N- (2-hydroxyethyl)-ethylene- diamine are then metered in over the course of 3 hours, during which the water of reaction formed is collected in a water separator and distilled off (about 29 parts). After the addition of the amine, the reaction is allowed to continue for 60 minutes at 180°C, and evacuation to 100 mbar is effected. After I hour, the product is cooled to 80°C and discharged.

1.2 Production of amide (Bl) 324 parts of stearic acid, technical grade (acid number 207.5) (mixture of stearic acid and palmitic acid), are heated to 100°C under nitrogen. 134.6 parts of 3-dimethylamino-1-propyl- amine are then allowed to run in, during which the temperature is held at between 100 and 110°C.

After the addition of the amine, the reaction mixture is heated to 130°C over the course of 60 minutes and, after 3 hours at 130°C, it is heated to 180°C over the course of 6 hours. After 5 hours at 180°C, evacuation is effected to a residual vacuum of 60 mbar, and the product is then cooled to 100°C and discharged. During the condensation reaction, about 12.2 parts of amine distil off together with 21.6 parts of water.

1.3 Production of dispersion (W ;) 108.3 parts of condensate (Al) and 21.7 parts of amide (B I) are mixed with one another, heated to the melting point, stirred and shaped to pellets (pelleted) and cooled. 130 parts of this pellet-form

mixture are added with stirring to a solution of 19.5 parts of glacial acetic acid in 773.5 parts of water. After the heating to 60°C, stirring is continued at this temperature for a further 60 minutes and then there is cooled to room temperature. A fine, highly fluid dispersion forms which is mixed firstly with 75 parts of polyethylene glycol 200 and subsequently with 1 part of Silikon Antischaumemulsion SE 2 (Wacker Chemie, Germany) and with 1 part of Saniprot 9408 (Sanitized, Switzerland). The composition obtained is discharged. 1000 parts of dispersion (W,) are obtained.

Example 2 2.1 Production of condensate (A71 The procedure is as described in Example 1. 1, with the difference that instead of the 435 parts of technical-grade stearic acid, 435 parts of pure stearic acid (90-95 %, by gas chromatography) (acid number 196.8), and instead of 98 parts, 93.6 parts of N- (2-hydroxyethyl)-ethylenediamine are employed, and about 27.5 parts of water of reaction are distilled off.

2.2 Production of amide (B) The procedure is as described in Example 1.2, with the difference that instead of the 324 parts of technical-grade stearic acid, 324 parts of pure stearic acid (90-95 %, by gas chromatography) (acid number 196.8), and instead of 134.6 parts, 127.8 parts of 3-dimethylamino-1-propylamine are employed, and about 11.6 parts of amine are distilled off together with 20.5 parts of water.

2.3 Production of dispersion (W} The procedure is as described in Example 1.3, with the difference that instead of the 108.3 parts of condensate (Al) and 21.7 parts of amide (Bl), 108. 3 parts of condensate (A2) and 21.7 parts of amide (B2) are employed.

Example 3 3.1 Production of condensate (A) The procedure is as described in Example 1.1, with the difference that instead of the 98 parts of N- (2-hydroxyethyl)-ethylenediamine, 111. 7 parts thereof are employed.

3.2 Production of dispersion (W) The procedure is as described in Example 1.3, with the difference that instead of the 108.3 parts of condensate (Al) and 21.7 parts of amide (Bl), 108.3 parts of condensate (A3) and 21.7 parts of amide (B2) are employed, and instead of polyethylene glycol 200, polyethylene glycol 400 is employed.

Example 4 4.1 Production of condensate (A41 The procedure is as described in Example 1. 1, with the difference that instead of 98 parts of N- (2-hydroxyethyl)-ethylenediamine, 88.2 parts thereof are employed.

4.2 Production of dispersion (W4) The procedure is as described in Example 1.3, with the difference that instead of the pellet-form mixture of 108.3 parts of condensate (Al) and 21.7 parts of amide (BJ, a pellet-form mixture of 108.3 parts of condensate (A4) and 41.7 parts of amide (B) are employed and, instead of a solution of 19.5 parts of glacial acetic acid in 773.5 parts of water, a solution of 19.5 parts of glacial acetic acid in 753.5 parts of water is employed.

Example 5 5.1 Production of condensate (A and amide (Bs) as a mixture 512 parts of stearic acid, technical grade (acid number 207.5) (mixture of stearic acid and palmitic acid), are heated to 100°C under nitrogen. 32 parts of 3-dimethylamino-1-propylamine are then allowed to run in, during which the temperature is held at between 100 and 110°C. After the addition of the dimethylaminopropylamine, the reaction mixture is heated to 130°C over the course of 60 minutes and, after 3 hours at 130°C, it is heated to 180°C over the course of 6 hours.

98 parts of N- (2-hydroxyethyl)-ethylenediamine are then metered in over the course of 3 hours, and the reaction is allowed to continue at 180°C for 60 minutes, and then evacuation is effected to a residual vacuum of 100 mbar. After 1 hour at 180°C and 100 mbar, the mixture is cooled to 80°C, the vacuum is released with nitrogen and the produced mixture is discharged. During the condensation reaction, a total of about 37 parts of distillate form, consisting of about 34.1 parts of water and 2.9 parts of dimethylaminopropylamine.

5. 2 Production of dispersion (Ws) 130 parts of the produced mixture of condensate (A5) and amide (B5) are heated to the melting point and shaped to pellets (pelleted) and cooled. 130 parts of this pellet-form mixture are added with stirring to a solution of 19.5 parts of glacial acetic acid in 374.5 parts of water. After heating to 60°C, stirring is continued at this temperature for a further 60 minutes, and 399.5 parts of water and subsequently 75 parts of polyethylene glycol 200 are added dropwise. The mixture is then cooled to room temperature. A fine, highly fluid dispersion forms, which is then mixed with 1 part of Silikon Antischaumemulsion SE 2 (Wacker Chemie, Germany) and 1 part of Saniprot 9408 (Sanitized, Switzerland). The resultant composition is discharged. 1000 parts of dispersion (W5) are obtained.

Application Example A 1 kg (dry weight) of the substrate to be finished (cotton single jersey, dyed blue with 3.1 % of C. I.

Reactive Blue 52, then washed and rinsed) are treated with 40 g of dispersion (WI), at 40°C, in an aqueous liquor at a goods-to-liquor ratio of 1: 8 in a Mathis (Switzerland) laboratory jet. The liquor circulation is 60 1/min and the treatment time is 30 minutes. The water has a hardness of 10° dH (in accordance with DIN 53905). The pH of the liquor is 5 (set with glacial acetic acid).

After the treatment, the treated goods are centrifuged, dried at 140°C for 90 seconds without tension, and the soft handle of the goods is determined. No deposits occur during the treatment.

No spots are evident on the textile goods. After the liquor has been let out, no residues can be observed in the machine. A significant improvement in the soft handle of the finished goods is achieved.

Application Example B 1 kg (dry weight) of the substrate to be finished (cotton woven fabric) is introduced into a Mathis (Switzerland) laboratory jet in 10 1 of water of 10° dH. A solution of 12 g of C. I. Direct Violet 66 in 1 1 of water is then added to the bath, and the bath is heated to 95°C at a liquor circulation of 60 I/min. On reaching this temperature, 1000 g of a 15 % sodium sulphate solution are added over the course of 20 minutes, and the dyeing is carried out at constant temperature for a further 30 minutes. After cooling to 70°C, the batch is let out, and the goods are rinsed a number of times (3 times) hot and cold. After the final rinse water has been let out, 8 1 of cold water (10°dH) are then loaded, and the pH is adjusted to 6 with acetic acid. 40 g of dispersion (W) are then added, and, at the same circulation rate of 60 I/min as during dyeing, the bath is heated to

40°C and treatment is continued at this temperature for 30 minutes. After this treatment, the clear, completely exhausted bath is let out, and the treated goods are centrifuged and dried at 140°C for 90 seconds without tension. No spots are evident on the textile goods. No deposits were observed in the Mathis laboratory jet. A significant improvement in the soft handle of the finished goods is achieved.

Each of dispersions (W2), (W3), (W4) and (Ws) is employed analogously to dispersion (W) in Application Examples A and B. All dispersions (WI) to (W5) are shear-stable and give a significant improvement in the soft handle of the treated goods.




 
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