DE3334575A1 - Aqueous wax dispersions, their preparation and use - Google Patents

Abstract

Aqueous dispersions of non-oxidised paraffin waxes, using specific surfactants, have a high stability under severe and heterogeneous dynamic stress and are suitable for the finishing of fibre material, in particular for the finishing of textile material, above all for improving sewability and especially for application from aqueous medium in jet-dyeing equipment.

Description

Aqueous wax dispersions, their production and use

As end finishing for textile material, be it threads, be it webs of fabric or other textile products, is often a lubricant finish from an aqueous medium carried out, whereby it is often desired to equip with non-oxidized paraffins (Paraffin wash). It is usually difficult to put non-oxidized paraffins in a To bring a stable, dispersed, easily dilutable form with water, and a special one The problem in textile technology is the production of aqueous paraffin wax emulsions, which even with high and heterogeneous, dynamic loads, such as in the jet dyeing machines, are stable.

It has now been found that using certain cation-active Surfactants, aqueous dispersions of non-oxidized paraffin waxes are produced can, specifically as they meet the requirements mentioned above.

The invention first relates to aqueous dispersions containing wax and surfactants, which are characterized in that the waxes are non-oxidised paraffin waxes with a dropping point of # 30 ° C. and the surfactants are cationic dispersants corresponding to the formula where R1 is a radical of the formula Rx-CO-O-, Rx-CO-NH- or Ry-O-, Rx alkyl or alkenyl with 7 to 21 carbon atoms, Ry alkyl or alkenyl with 8 to 22 carbon atoms or a radical er formula R 'is hydrogen or C1-9-alkyl, R "is C412-alkyl, R2 and R3 are each hydrogen, benzyl or a radical of the formula - (- CH2-CHOH-CH2-O-) p- - (- Alkylen3-O-) q-Rs (b), R4 hydrogen or a radical of the formula (b), R5 in each case a radical of the formulas - (- Alkylene4 ~ O -) - r-RZ (c), - (- Alkylene4-O -) - s -CO-RW (d) or -Alkylen4-NH-CO-RW (e), Rw alkyl or alkenyl with up to 21 carbon atoms, Rz alkyl or alkenyl with up to 22 carbon atoms or a radical of the formula (a), alkylen1 ethylene -1,2 and / or propylene-1,2, alkylene2 an alkylene bridge member with 2-6 carbon atoms, alkylene3 and alkylene4 each ethylene-1,2 and / or propylene-1,2, m 0 to 4, n 2 to 20, p, r and s each represent 0 or 1, and q represent 0 to 19, where p + q + s # 1, and when Rz represents a radical of the formula (a), p + q + r # 1, and optionally in protonated and / or quaternized form.

As the non-oxidized paraffin waxes, there are generally any Paraffin waxes can be considered, as they come from the processing of fossil hydrocarbon mixtures can arise. As fossil hydrocarbon mixtures are here in general Crude oil, bitumen, asphalt, tar and fossil coal (especially lignite) meant, the main sources being brown coal and, above all, crude oil. The paraffin waxes can mainly come from processing by distillation and, if necessary, from refining of fossil hydrocarbons, especially from distillation of petroleum. Primarily n-paraffins and isoparaffins come into consideration, like them in the processing or distillation of the heavier oil fractions, in particular Gas oil and lubricating oil, are available; from spindle oil and from light and medium viscosity Machine oil, paraffin waxes can be obtained9 which are richer in n-paraffins, while from heavy machine oil and from the cylinder oil distillation residues Paraffins are obtained which are richer in isoparaffins and optionally cycloparaffins are; the paraffin waxes are initially obtained in an oily form, e.g. as Gatsche or as petrolatum or Vaseline. The muds can be refined especially if they are as low in isoparaffin as possible, and it can be made from the lighter ones very pure n-paraffin waxes can also be obtained from the above-mentioned oil fractions (table paraffin), which can have an n-paraffin content of up to 93%. Isoparaffin-rich mace are more difficult to refine, but can still be partially de-oiled. Have petrolatum a high isoparaffin content and petroleum jelly and micro-waxes can be obtained from it will.

Very pure n-paraffin waxes can be used for the preparations according to the invention or very pure isoparaffins (micro waxes), as well as mixtures thereof, are used; the waxes or wax mixtures used can advantageously also contain oil, although the oil content should preferably not be so high that the Oil exudes from the wax by itself; the oil content is advantageously that according to the invention Waxes to be used values' 30% by weight. In particular, hard paraffins or Soft paraffins can be used or low-oil paraffin waxes with appropriate middle and / or heavier mineral oil fractions (boiling point higher than 250 ° C) or it can be low-oil paraffin waxes with others oil richer Paraffins, e.g. with petrolatum, slash or petroleum jelly. The oil content of the waxes or wax mixtures to be used according to the invention is advantageously 0 to 30%, preferably 0.2 to 15%, with waxes richer in isoparaffin the higher ranges of oil content are preferred, while the higher ranges of n-paraffin The lower oil content ranges, in particular <5%, grow preferentially are. Paraffin waxes are particularly preferably used, which are both n-paraffins as well as isoparaffins, the n-paraffin content advantageously being 30 to 90 % By weight, preferably 65 to 90% by weight, in particular 80-90% by weight of the wax used matters. Technical mixtures or raw products can also be used, which contain both n-paraffin waxes and isoparaffins and possibly oil, such as isoparaffin-containing satchel, n-paraffin waxes cut with petrolatum or or refined garlic cut with micro-waxes or ceresins or Soft paraffins. Practically oil-free or low-oil n-paraffin waxes are particularly preferred used, whose n-paraffin content is 5 65%, preferably 80%.

The solidification points of the paraffin waxes or paraffin wax mixtures used can vary within a wide range, advantageously between 40 and 100 ° C., preferably between 50 and 65 "C.

The needle penetration according to ASTM D 1321 can also be within a wide range vary and, according to the invention, non-oxidized waxes or

Wax mixtures are used which allow needle penetration, e.g. in the range from 5 to 150, advantageously 20 to 140; preferably be Hard paraffins are used, especially those with needle penetration according to ASTM D 1321 in the range from 10 to 30.

The acid number of the waxes used corresponds to that of non-oxidized Wake up, i.e. it is <1, preferably <0.5.

The oils and waxes mentioned are e.g. in Carl Zerbe "Mineral oils and related products ", Springer-Verlag, (2nd edition, 1969), especially in the second and in the eighth chapter.

The cation-active dispersants to be used according to the invention contain at least an amine-bonded radical of the formula RlfAlkyl enl-OCH2-CHBH CH2 (a) and can im aqueous medium, optionally in protonated and / or in quaternized form The remainder Rx advantageously contains 11 to 21, particularly preferably 15-19, Carbon atoms, in general the alkyl radicals and among the alkenyl radicals the oleyl radical are preferred.

The alkyl and alkenyl radicals in the meaning of Ry advantageously contain 12 to 22, 16-22, particularly preferably 16-20 carbon atoms; in the formula (a) the radical R ″ is preferably in the para position; the sum of the carbon atoms in R 'and R "is advantageously 8 to 12; R' is preferably hydrogen or n-, iso- or tert-butyl and R ″ preferably denotes C4-6 alkyl, especially radical (a) is preferably dibutylphenyl or octyl- or nonylphenyl. Ry is advantageously C16-22 alkyl or alkenyl, preferably C16-20 alkyl or alkenyl, especially stearyl or oleyl.

Of the Alkylen1 radicals are advantageously at least 50 mol% of ethylene - 1.2, where preferably all alkylene bridge members are ethylene bridge members. Of the The index n advantageously stands for 3 to 12, preferably for 4 to 8.

The alkylene2 bridge member advantageously stands for 1,2-ethylene, 1,3-propylene or 1,6-hexylene, of which 1,2-ethylene and in particular 1,3-propylene are preferred The index m advantageously stands for 0, 1 or 2, preferably for 1 The alkylene bridge members Alkylen3 and Alkylen4 are advantageously 1,2-ethylene and / or 192-propylene, where preferably at least 50 mol% of the alkyleneoxy bridge members occurring in remainder (b) Are ethyleneoxy; particularly preferably all alkylenes3 and all alkylenes4 denote 1,2-ethylene.

The radicals of the formula (b) are preferably alkyl or alkenyl with up to 22 carbon atoms or a radical of the formula (a). The molecule of the formula (I) preferably contains at least one nitrogen-bonded alkyl or alkenyl radical having 8 to 22 carbon atoms, this substituent preferably being the substituent R4; More than just one radical of the formula (a) is advantageously present in the molecule and at least one of the radicals R2 and R3 is particularly preferably a radical of the formula (a); the symbols R2, R3 and R4 can also mean hydrogen, but preferably at least one of the substituents R2 to R4 is different from hydrogen; those of the substituents R2 to R4 which are not a radical of the formula (a) and are also not alkyl or alkenyl having 8 to 22 carbon atoms can, for example, also be benzyl or C1-4-, preferably C1-2-alkyl. In the cationic surfactants, in addition to the nitrogen-bonded radicals of the formula (a) and optionally, in addition to nitrogen-bonded hydrogen, only nitrogen-bonded alkyl or alkenyl radicals having 8-22, advantageously 16-22, in particular 16-20 carbon atoms, are preferably present; the radicals of the formula (a) occurring in the molecule preferably correspond to the formula -CH2-CHOH-CH2-0- + CH2-CH2-O t Ryt (a '), in which Ryl is C822-alkyl or alkenyl or a radical of the formula R01 is n-, iso- or tert-butyl or hydrogen and n1 is 3 to 12; the radicals particularly preferably correspond to formula (a) or

(a ') of the formula -CH2-CHOH-CH2-O4CH2-CH2-0 n Ryl (a ") wherein Ry is C16-22 alkyl or -alkenyl and n2 are 4 to 10; Ry is particularly preferably alkyl or Alkenyl having 16 to 20 carbon atoms and the index n2 preferably stands for 5 to 8.

The cation-active surfactants of the formula (I) preferably correspond to the formula wherein R21 and R3 'are each hydrogen, C1,2-alkyl or a radical of the formula (a'), R41 is C822-alkyl or alkenyl or a radical of the formula (a '), m1 is 0 to 2 and x is 2 or 3 ; of which those of the formula and especially those of the formula where R2 "and R3" are each hydrogen or a radical of the formula (a ") and R41, C16-22-alkyl or alkenyl, where at least one of R2" and R3 "is a radical of the formula (a"), are preferred .

Ry'3 is particularly preferably Ryll, R4 'and R41 in the above Formulas alkyl or alkenyl with 16 to 20 carbon atoms and n1 and n2 5 to 8.

The cationic surfactants can be in protonated form, what can generally be achieved by adding common acids, e.g.

Hydrochloric acid or sulfuric acid or low-molecular, aliphatic Acids, e.g. formic acid, acetic acid, tartaric acid or citric acid, of which in particular formic acid and especially acetic acid are preferred.

The cationic surfactants can optionally be used in quaternized form are present, i.e. at least one of the basic nitrogen atoms occurring in the molecule is quaternized; the quaternization gives preference to ethyl or methyl radicals introduced, as well as corresponding counterions, primarily halide (chloride, bromide, Iodide), methosulphate or ethosulphate.

Among the surfactants to be used, however, are the non-quaternized ones preferred.

A particular subject of the invention are those defined above Compounds of the formulas (I), (I ') and (I "), which are optionally in protonated and / or quaternized form and in which R4 and R41 are alkyl or alkenyl with Mean 8 to 22 carbon atoms.

The surfactants mentioned can be produced in a manner known per se will; a preferred process for the preparation of the compounds of formula (I), optionally in protonated and / or quaternized form, is characterized by that a compound of the formula H2N-4Alkylen2-NH + Rl4 (II) in which R14 is hydrogen or alkyl or alkenyl with up to 22 carbon atoms or a radical of the formula (e) means, with corresponding, radicals of the formula (a) and optionally of (a) and (e) various radicals of the formula (b) and / or compounds which donate benzyl radicals converts and optionally protonated and / or quaternized.

As the radicals (a) or (b), where p = 1, donating compounds, in particular the corresponding halides (especially chlorides and bromides), as well as the corresponding epoxides are mentioned; for the benzylation are preferred Benzyl chloride or benzyl bromide used for introducing radicals of the formula (b), where p = 0, are preferably corresponding halides, preferably Chloride or bromide used. To introduce the radicals of the formula (a) are preferably the halides of the radicals of the formula (a) to the corresponding epoxides dehydrohalogenated and then the corresponding epoxides are attached to them Amines of the formula (11) added on; are in the molecule from the existing residue R14 and from If you want radicals different from radicals (a), then these can then be reacted be introduced with appropriate reagents.

The halides are converted into the corresponding epoxides in a manner known per se, advantageously using alkali metal hydroxides (preferably sodium hydroxide) in an aqueous medium in the heat, advantageously in the Temperature range from 30 to 80 "C; the epoxy can be in the same aqueous medium be reacted with the amine of the formula (II), advantageously in the heat, preferably in the temperature range from 50 to 1000 ° C., preferably 60 to 80 ° C. The Water can then be removed by distillation and the resulting salts can pass through Hot filtration of the anhydrous product can be removed at temperatures above the melting point of the corresponding surfactants, e.g. between 70 and 100 "C. If desired, they can be protonated with customary acids and / or with customary Quaternizing agents are quaternized; come as acids for protonation the above mentioned; as quaternizing agents are preferably methyl and ethyl halides (preferably bromides or iodides), diethyl sulfate and dimethyl sulfate into consideration. The quaternization is generally carried out in the usual manner, optionally in an aqueous, aqueous / organic or organic medium in which Warmth (e.g. at 40-100 ° C).

Preferably the non-quaternized and non-protonated Bases used as such and only during the preparation of the aqueous dispersion protonated.

In the aqueous wax dispersions according to the invention, the cation-active The dispersant is expedient at least in such a proportion to the paraffin wax used as it is sufficient to disperse the paraffin wax in the water; the Cation-active surfactant can also be used in excess. Advantageous are at least 20, preferably 20, per 100 parts by weight of the paraffin wax up to 150, in particular 40 to 120 parts by weight of the cationic dispersant are used (with higher n-paraffin content, higher surfactant content is preferred are; so for at least 65% n-paraffin at least 50% surfactant and for at least 80% n-paraffin at least 80% surfactant). The amount of water used is appropriate at least as much as is sufficient for the dispersion to be stirrable or pourable; It is advantageous to use enough water that the dry matter content of the dispersion at most 50% by weight, preferably 5 to 50% by weight, in particular 10-30% by weight. The pH of the dispersion becomes particularly advantageous by adding an acid to values between 3 and 6, preferably between 3 and 4.5, set, the cation-active Dispersants are advantageously used as free bases, so that in the dispersion the corresponding protonated form is created. If necessary, the inventive Dispersions still contain a common cold stabilizer, e.g. a water-soluble one monohydric or polyhydric alcohol (e.g. isopropanol, ethylene glycol, hexylene glycol or glycerine) or a water-soluble polyalkylene glycol or a water-soluble one Mono- or polyalkylene glycol alkyl ethers (e.g. diethylene glycol, methyl cellosolve or Ethyl cellosolve).

In a preferred composition of the wax dispersions according to the invention are per 100 parts by weight of the non-oxidized aliphatic paraffin wax a Parts by weight of the cationic dispersant, b parts by weight of an acid, c parts by weight Water, and d parts by weight of a cold stabilizer, in which a 20 to 150, is preferably 40 to 120, b is used to adjust a pH value of 3 to 6, is preferably 3 to 4.5 necessary amount of an acid, c is the setting of a Dry matter content of 5 to 50% by weight, preferably 10 to 30% by weight, necessary Amount of water and d is 0 to 40% by weight of c, preferably 5 to 20% by weight of c, in particular 7 to 15% by weight of c.

As far as paraffin wax is mentioned in this text with regard to the dispersions istg not only means a pure paraffin, but also paraffin wax mixtures, how they ultimately overall for the preparation of the dispersions according to the invention be used; also when speaking of a cationic dispersant, does not only mean a single compound, but also mixtures of compounds, as they e.g.

also arise during the production of the dispersants (the high molecular weight Fat residues in the surfactants can come from technical mixtures, the ethoxylation products are mostly mixtures and when reacted with primary amines or with polyamines can optionally have a different number of nitrogen-bonded hydrogen atoms can be converted by the appropriate reagent). If appropriate, acid mixtures can also be used can be used and the low-temperature stabilizers can optionally also be mixtures be.

The cation-active surfactants are advantageously found in the aqueous dispersions as salts, i.e. in quaternized or preferably protonated form.

The dispersions according to the invention can be prepared in a manner known per se e.g.

are made by mixing the respective ingredients together; The paraffin waxes are preferably fused with the appropriate dispersants and the melt is then with water and optionally with acid and / or with Cold stabilizer mixed; if an acid is to be added, this is preferred dissolved in the water before adding the melt, preferably during the cold stabilizer is only added after the formation of the dispersion. The wax dispersions according to the invention are free from oxidized waxes and have a high storage stability, i.e.

they remain in a well-dispersed form for a long time, and, if they should separate into layers after a certain period of time, they can brought them into their original, well-dispersed form by simply stirring them will.

The dispersions according to the invention serve as finishing agents for fiber material, especially textile material, preferably as a lubricant or softeners, and are a special subject of the invention watery Finishing agent for fiber material, which by a content of non-oxidized Paraffins and cation-active dispersants, as defined above and in particular are also preferred, as well as the use of the above-defined, aqueous wax dispersions as finishing agents for fiber material and the process for finishing fiber material, which is characterized in that one for it aqueous dispersions or

aqueous finishing agents as defined above and particularly preferred, optionally in a form diluted with water.

Suitable for finishing with the finishing agents according to the invention any fiber materials, as they are usually equipped with paraffins materials, both natural and synthetic and semi-synthetic and their mixtures, in particular natural or regenerated cellulose, natural or synthetic polyamide, polyester, polypropylene and polyacrylonitrile containing Material and mixtures thereof. The material can be processed in any form present, e.g. as loose fibers, filaments, threads, yarns, strands and spools of yarn, Woven fabrics, knitted fabrics, nonwovens, nonwovens, paper webs, felts, carpets, velvet, tufted goods or semi-finished goods and also artificial leather. Particularly noteworthy among them is the waxing of paper webs, the wet waxing of bobbins and especially the finishing of textile webs.

The finishing is advantageously carried out using aqueous, preferably acidic Me medium, favorably at pH values between 3.5 and 6, preferably between 4 and 5.5 (adjusted e.g. by adding an acid common in dyeing technology, such as formic acid, acetic acid, citric acid or tartaric acid) and in a temperature range, which is generally compatible with the substrates used, advantageously between 10 ° C and 60 "C, preferably between 30 and 50" C, using exhaust or impregnation processes. Any customary processes are suitable as impregnation processes, e.g. immersion, padding, Foam or spray processes, in particular also continuous processes, depending on the substrate and equipment used. The finishing agents according to the invention have a good one Substantivity and are not only suitable for impregnation processes but also for exhaust processes; as an exhaust process, any process come from both long and from a short fleet in Consider advantageous with a liquor ratio from 1: 100 to 1: 0.5, in particular between 1:60 and 1: 2, with the short liquor method in particular the processes in the reel curve and, above all, in the nozzle dyeing machines (dye-jet machines) are to be emphasized. The treated substrate becomes beneficial directly dried without subsequent rinsing; you can view the treated material let it dry in the open air or, advantageously, at a higher temperature, e.g. in a temperature range between 80 and 1500C (such as in a conventional drying cabinet) dry. The concentration of the waxes, based on the substrate, can, depending on Type and texture of the substrate and the desired effect, within wide limits vary and is advantageously values between 0.02 and 1.5, preferably 0.1 up to 0.8%, based on the dry weight of the substrate.

Since the dispersions according to the invention even at high and heterogeneous, dynamic loads are very stable, they are particularly suitable for Finishing of textile webs in nozzle dyeing machines. As nozzle dyeing machines Any customary apparatus, such as those used in technology and in the literature, is suitable are known, e.g. in the following: - Anonymous: Review of the 6th ITMA 1971 in Paris, Textilveredlung 6 (1971) 11, pages 745-748.

- P. Semer: ITMA 75 - dyeing and textile finishing. Melliand textile reports 57 (1976) 2, pp. 147-149.

- R.D. Holt, F.J. Hassigan: The failure of piece goods in jet and overflow dyeing machines; Melliand Textile Reports 60 (1979) 9, pages 745-758.

- W.J. Marshall "Jet Dyeing Machines (Process development and machinery review) ", Shirley Institute Publication p. 33 (The cotton, silk and man-made fibers research association, 1979).

The usual "laboratory jets" can also be used for experimental purposes e.g. Mathis Labor Overflow-Jet JFO from Mathis (Niederhasli / ZH, Switzerland).

The different jet dyeing machines cover a wide range dynamic stress on textile material and liquor, e.g. depending on the liquor circulation, Goods speed and liquor ratio, especially in the case of equipment that is not fully flooded. Different forces act in the different parts of the apparatus, so that E.g. the treatment liquor in different places very strong speed differences and in this apparatus, for example, strong shear forces can and also act more or less stable foam can arise, so that when using unstable Wax dispersions wax can float out, and when unloading the treated textile goods some of the wax that has floated out sticks and the There are wax grease stains on it. The dispersions according to the invention have a high stability even with such high dynamic loads, see above that the effectiveness of the finishing agent is optimally used and the substrate is equipped as regularly as possible.

The stability of the dispersions according to the invention can be determined in a simple manner Way to be checked in the laboratory by placing the dispersions in an apparatus are subjected to such dynamic stresses as in jet dyeing machines can occur using a running at high speed Knife Quirles. Such fast-running, electrically driven knife whisks are generally known and, for example, the usual mixers in the household, e.g. the household mixer type MX 32 from BRAUN A.G. (Frankfurt am Main). The stability of the dispersions can be tested as follows, for example: 5g of the The dispersion is made up to 1 liter with demineralized water. For 2 determinations 1/2 liter of the diluted dispersion are poured into the mixing vessel of a household mixer, Type MX 32 from BRAUN A.G.

(Frankfurt am Main), (idling speed at stage III = 16,000 + 10% Rpm at an idle consumption of 205 W i 10%) and on level III whisked very vigorously for 1 minute.

The dispersion treated in this way is then subjected to a suction vacuum of 530 mbar through a suction filter (diameter = 5.7 cm) with a layer of commercially available black Cotton cretonne (130 g / m2, 16 weft threads and 17 warp threads per cm2) filtered.

Afterwards, dispersions show stable against high dynamic loads no or only a negligible filtering off of white paraffin.

By using hard water (e.g. 10 ° dH) and / or increasing it The concentration dispersion per 1 liter of water can tighten the examination conditions will.

The finishing agents according to the invention influence the colorations or lightening of the substrates. They are especially for dealing with cellulosic knitwear, especially cotton knitwear.

In the following examples, parts mean parts by weight and Percentages by weight, the temperatures are given in degrees Celsius.

Paraffin waxes used a) Arco Wax 4154 G [supplied by: Arco Raffinerie GmbH, Hamburg, Germany] b) Arco Wax 1150 G [do] c) Arco Wax 2143 G, batch 1878 [do] d) Petrolatum, light amber technical [supplied from: Witco Chemical, Sonneborn Division, Koog aan de Zaan, NL] e) Arco Wax 4158 G [supplied by: Arco Raffinerie GmbH, Hamburg, Germany] with the following properties: Solidification dropping point needle penetration oil content n-paraffin Wax point in ° C, in ° C after after after content after according to M-III 3 (75) * ASTM D 1321 ASTM D 721 MV 8 (63) * ASTM D 87 a 54/56 55.9 Ku 20 t- 0.5% 80-84% b 50/52 53.6 nr 80 3-4% 68-70% c 43/45 48 ~ 130 ~ 3% 70-78% d 48/56 51-57 160-180 19-22% (Cone penetration) e 58/60 58.9 || ~ 20 # 0.5% 88-90% * DGF standard methods for the investigation of fats, fat products and related substances, from the German Society for Fat Science eV, Münster, Westf., In the Scientific Publishing Catalog, Stuttgart, 1982.

Surfactants used Compounds of the average formulas Surfactant | Formula | R24 | R11 | t + u + v + w A (2) R241 C18 H37 t + u + v = 18 B (3) R24 '"t + u + v + w = 24 C (2) R24 "" t + u + v + w = 18 D (2) R24 "'" t + u + v + w = 18 E (1) R24 'C18 H35 t + u = 12 F (2) R24 '"t + u + v = 18 wherein R24t a mixture of R2411 a mixture of and R24.11 a mixture of 0.1% C12H25- 3.0% C8 H17- 1.3% C14H29- 0.9% C14H29- 6.0% C10H21- 4.7% C16H33- 28.0% C16H33- 56.0% C12H25- 42.0% C18H37- 28.0% C18H37- 18.0% C14H29- 12.0% C20H41- 43.0% C18H35- 10.0% C16H33- 40.0% C22H45- 2.0% C18H37- 5.0% C18H35- are.

Preparation of the wax dispersion Regulation 1 156.7 parts of paraffin wax and 84.3 parts of surfactant are melted together and, with stirring, in a to 70 ° heated solution of 855 parts of demineralized water and 15 parts of glacial acetic acid entered. The fine emulsion obtained in this way is cooled with further stirring relaxed and still at 95 Parts of ethylene glycol are added. Thereafter the milky, thin liquid dispersion is unloaded. (According to this provision are the dispersions of Examples 1, 2, 3, 4, 5 and 6 below).

Regulation II Proceed as in regulation I, but use 172 Parts wax, 69 parts surfactant, 940 parts water and no ethylene glycol.

The dispersions of the examples below follow this rule 7, 8 and 9 made.

Regulation III 60 parts of surfactant and 60 parts of paraffin wax are melted together and while stirring in a heated to 85 "solution of 425 parts of demineralized Entered water and 15 parts of glacial acetic acid. The very fine emulsion thus obtained is allowed to cool and then 47 parts of ethylene glycol are added. Thereafter the almost clear, opalescent, thin-bodied dispersion is unloaded. After this The dispersions of Examples 10, 11 and 12 are prepared according to the instructions.

Regulation IV Proceed as in Regulation II, but now use 855 parts of water.

According to this specification, the dispersions of Examples 13, 14 and 15 manufactured.

Regulation V The procedure is as in Regulation II, but instead of the 940 parts of water, 855 parts of water and then 95 parts of ethylene glycol are used. The dispersions of Examples 16, 17 and 18 were prepared according to this procedure. Example p surfactant | Waxes (weight ratio) 1 A c - 2 A c + d (9: 1) 3 E b + d (6: 4) 4 F b + d (6: 4) 5 A a + d (6: 4) 6 A e + d (7: 3) 7 D b + d (7: 3) 8 C b + d (9: 1) 9 B b + d (7: 3) 10 A a 11 A e 12 A b 13 D b + d (7: 3) 14 C b + d (9: 1) 15 B b + d (7: 3) 16 D b + d (7: 3) 17 C b + d (9: 1) 18 B b + d (7: 3) The dispersions produced in Examples 1-18 are stable in storage and no paraffin deposits are found in the "mixer test" described above (5 g of dispersion per 1 liter of demineralized water whisked for 1 minute and filtered through a black cloth filter).

The black fabric filter used is manufactured as follows: bleached Cotton cretonne (130g / m29 16 weft threads and 17 warp threads per cm2) is used with liquor ratio 1:40 for 30 minutes at 60 to 70 ° with 6% C.I.

Direct Black 19 colored and then with 2% 35% formaldehyde and 2% Treated with glacial acetic acid and finally rinsed thoroughly and dried. Of the black-dyed cotton cretonne pieces in the required size for the inserted filter punched out.

Preparation of Surfactants A-F Surfactant A is prepared as follows 135 parts of stearyl alcohol are catalysis of 0.4 by a known method Parts of caustic soda added on to 132 parts of ethylene oxide, followed by 46.5 parts of epichlorohydrin with catalysis of 4 parts of about 48% boron trifluoride dietherate at one temperature between 45 and 70 ". The chlorohydrin formed is then added with 60 parts of 30% strength Sodium hydroxide solution converted into the epoxy at 40-50 °, which continues for 5 hours at 70 is reacted with the fatty amine R24'-NH-CH2CH2CH2-NH2 (for the meaning from R24 ': see the table of surfactant formulas). Then the existing Water is removed by distillation and the sodium chloride formed is removed by filtration at approx. 80 ". The surfactant obtained in this way solidifies at room temperature.

All work steps in this example can be carried out continuously without intermediate isolation be carried out in a working vessel.

The surfactants B to F are produced in an analogous manner.

Application example A A length of 200kg cotton interlock (200g / m2) is used in a Thiess-Jet R 95 with 3 units (3 curves) with 1600 liters Liquor containing 6kg of the dispersion according to example 1 (= liquor ratio 1: 8), for 20 minutes, at 45 "and with a circulation of 180 m / minute; without The finished goods are subsequently rinsed in the drying cabinet at 110 to 1200 dried and then ready to use.

Application example B Cotton interlock is made at 40 ° and a liquor ratio 1:40 in an aqueous liquor that, based on the substrate, 3% of the wax dispersion according to Example 3, after 20 minutes at 40 ° with constant movement of the substrate this is taken from the liquor and dried for 90 seconds at 140 ° without tension. Alternately, the wax dispersion can only be added when the substrate is already in the aqueous liquor.

Application example B1 to B7 Proceed as described in example B, but uses the same concentration instead of the dispersion according to Example 3 of the dispersion according to Example 4, Example 7, Example 8 or Example 9 or 2% the dispersion according to Example 1, Example 2 or Example 10.

Application example C Cotton interlock is made at room temperature padded with an aqueous liquor up to a 75% dry weight increase, which contains 30g / l of the wax dispersion according to Example 8. Then it will padded material dried for 90 seconds at 140 °.

Application examples C1 to C3 Proceed as described in example C, but uses the dispersion according to example instead of the dispersion according to example 8 3, 5 or 6 or 25 g / l of the wax dispersion according to Example 10.

Application example D In a Mathis Labor Overflow-Jet JFO the Company Mathis, Niederhasli / ZH, Switzerland, 1.0 kg cotton tricot interlock, pre-dyed tubular fabric 52 cm wide, 520 cm long, 185g / m2, in a liquor of 8 1 tap water (4-6 ° d.H.) with a liquor circulation of 14'700 l / h and one Goods speed of 23 m / min (nozzle diameter = 70 mm) 30 minutes at 25 ° treated with 55 g of the dispersion according to Example 10, and as in the application example A dried.

The product finished according to the above application examples shows no wax stains and is easy to sew.

Claims (11)

Claims: Claims: 1. Aqueous wax and surfactant-containing dispersions, characterized in that the waxes are non-oxidized paraffin waxes with a dropping point of \ 30 ° C and the surfactants of the formula where R1 is a radical of the formula Rx-CO-O-, RX-CO-NH- or Ry-O-Rx alkyl or alkenyl with 7 to 21 carbon atoms, Ry alkyl or alkenyl with 8 to 22 carbon atoms or a radical of the formula R 'is hydrogen or C1-g-alkyl, RI is C4 ~ l2-alkyl, R2 and R3 are each hydrogen, benzyl or a radical of the formula - (- CH2-CHOH-CH2-O-) p- - (Alkylen3-O-) q-R5 (b), R4 hydrogen or a radical of the formula (b), R5 in each case a radical of the formulas - (Alkylen4-O) r-Rz (c), - (- Alkylen4-O-) s-CO-Rw (d) or -Alkylen4-NH-CO-Rw (e), Rw alkyl or alkenyl with up to 21 carbon atoms, Rz alkyl or alkenyl with up to 22 carbon atoms or a radical of the formula (a), Alkylen1 ethylene-1,2 and / or 1,2-propylene, alkylene2 an alkylene bridge member with 2-6 carbon atoms, alkylene3 and alkylene4 each 1,2-ethylene and / or 1,2-propylene, m 0 to 4, n 2 to 20, p, r and s each 0 or 1, and q 0 to 19, where p + q + s I 1, and, if Rz is a radical of the formula (a), p + q + r # 1, optionally in protonated and / or quaternized form. 2. Concentrated, aqueous dispersions according to claim 1, containing 100 parts by weight of a non-oxidized aliphatic paraffin wax a parts by weight cation-active dispersant b parts by weight of an acid c parts by weight water d parts by weight a cold stabilizer in which a 20 to 150, b for setting a pH value from 3 to 6 necessary amount of an acid, c the setting a dry matter content of 5 to 50% by weight necessary amount of water, and d 0 to 40% by weight of c are. 3. Dispersions according to claims 1-2, wherein the wax is an n-paraffin, isoparaffin and oil-containing, non-oxidized paraffin wax. 4. Use of the dispersions according to Claims 1-3 as finishing agents for fiber material. 5. A method for finishing fiber material, characterized in that that, for this purpose, dispersions according to claims 1-3, if appropriate, are used as finishing agents used in form diluted with water. 6. The method according to claim 5, characterized in that according to equips the exhaust process. 7. The method according to claim 6, characterized in that in Jet dyeing machines. 8. The method according to claims 5-7, characterized in that one Textile material made from natural or regenerated cellulose, natural or synthetic Polyamides, polyester, polyacrylonitrile or polypropylene or mixtures thereof, disengages. 9. The material equipped according to claims 5-8. 10. Cation-active, surfactant compounds of the formula (I), defined as in claim 1, wherein R4 is alkyl or alkenyl having 8 to 22 carbon atoms, optionally in protonated and / or quaternized form. 11. Process for the preparation of the compounds according to claim 10, characterized in that a compound of the formula H2N- (Alkylen2-NH W R4 (II) with corresponding, radicals of the formula R1-CAlkylenl-0) 71-CH2-CHOH-CHZ- (a) and optionally donating radicals of the formula (b) and / or benzyl radicals different from (a) Reacts compounds and optionally protonated and / or quaternized.