DE864986C - Preparation and process for finishing textiles - Google Patents

Description

It is well known that textiles, such as fabrics, yarns, threads and fibers, are made with the most varied of types Agents treated to make them crease-proof and water-repellent and to prevent them from shrinking or matting to prevent. For this purpose oils, plasticizers, sizes, binders and others are used Materials are used, thereby improving the appearance, feel, etc. of the goods. Purpose of the invention is a method and a preparation to improve the properties of textiles, especially their resistance against water, the handle and the crease resistance of the same to improve significantly and to reduce their tendency to shrink.

The textiles used for the process according to the invention are fibers, threads, yarns, knitted goods, and woven fabrics Fabrics and others made of cotton, linen, hemp, jute, regenerated cellulose, cellulose ester, Cellulose ether, wool, synthetic wool, silk, rayon and other natural or artificial fiber materials into consideration. For the sake of simplicity, these textile materials are hereinafter referred to as textile fabrics designated.

. It is known that textile fabrics can be treated with aqueous dispersions of an alkylated methylolmelamine and to make them shrink-proof and crease-proof by subsequent drying. Those treated like that However, fabrics have an unsatisfactory hydrophobicity. In contrast, textile fabrics produced after Process according to the invention are obtained, in addition to the fastness to crease, fastness to shrinkage, a better one

Handle, etc. also has excellent water-repellent properties. Be for this purpose Textiles treated with an aqueous dispersion containing an alkylated methylolmelamine and certain substances containing nitrogen Contains substances. The resulting _ better results are probably due to certain conversions due, which during the drying ■ or the heat treatment between the alkylated methylolmelamine and the for use

ίο entering nitrogen-containing compound.

If a textile fabric, which with an alkylated Methylohnelamin, z. B. with methylated Methylolmelamine of the following formula

-c c — n:

CH ₃ OCH ₂ '

XH ₂ OCH ₃

_a5 - HN-CH ₂ OCH ₃

treated "is subjected to a heat treatment, polymerization occurs presumably one or more molecules of methyl alcohol undergoing molecular rearrangement that cause the polymerization favored, split off.

That the resulting fabrics are not particularly hydrophobic, in spite of the resin formation, is at least in part due to the fact that the resin formed during the polymerization of the methylolmelamine contains no effective hydrophobic groups. It's pretty easy to wet, with the Water also penetrates into the interstices of the tissue.

no Substituting compound of the class described hereinafter Methylohnelaminlösung other hand, a nitrogen-containing too, so the tissue occurs after the impregnation, drying and further treatment at relatively low temperatures vermut-Hch between the alkylated methylolmelamine and the nitrogen-containing compound a chemical reaction, which the The nature of the incorporated resin changes without, however, affecting the polymerization mechanism, which is necessary to achieve a permanently water-insoluble resin in the fabric.

According to the invention, as an N-containing compound any compound having a hydrophobic alkyl radical of at least 7 carbon atoms and a Has nitrogen atom to which an acidic group is attached, in connection with alkylated methylolmelamines be used. The union of such amido group-containing compounds with the alkylated Methylohnelamin takes place under the stated conditions by means of an active hydrogen atom, which is in the amido group or in a substituent, e.g. B. an alkylol radical, which with it is connected, present, is. Although other substituents are also present on the arnido nitrogen it should be mentioned that the compounds should be free of basic, salt-forming groups, since it was found that the hydrophobicity of Tissue is not permanent in the presence of such salt-forming groups. This disadvantage is possibly related to the water solubility of the salts formed in this way. It is therefore according to the invention it is desirable that the compounds be mainly acidic in character and not readily Able to form salts.

Of the amido group-containing compounds defined above, those which can preferably be used are have the following formula:

X O

I ii

Y_N-C-R

wherein Y is hydrogen or unsubstituted or substituted alkylol radicals, such as, for example, methylol or Ethylolradrkale, X and R hydrogen, non-reactive Substituents and radicals, which are hydrophobic alkyl groups of at least 7 carbon atoms have, mean. In all cases, at least one of the substituents X or R should be contain hydrophobic alkyl radicals of at least 7 carbon atoms.

It has been found that amides of the type represented by the formula H ₂ N -CO-R ', in which R' represents a higher alkyl radical, can be condensed with methylated methylolmelamines by heating the mixture on textile fibers, expediently in the presence of an acidic catalyst . The reaction probably takes place according to the following equation:

M-NH-CH ₂ -O-CH ₃ -IH-NH-CO-R '

> M - NH-CH ₂ -NH-CO-R '+ CH ₃ OH,

where M is the radical of the methylated methylolmelamine and R 'is a higher alkyl radical.

A similar reaction can take place on the fiber with methylated methylohnelamine and the aldehyde condensation product of an amide. It is known that aldehydes combine, e.g. B. formaldehyde, with amides to form methylol derivatives according to the following equation:

O: CH ₂ + H ₂ N-CO-R '

HO-CH ₂ NH-CO-R '.

The reaction between these compounds and the methylated methylolmelamines is likely take place as follows:

M-NH-CH ₂ -O-CH ^ _HO-CH2 -NH-CO-R '-> - ^ M-NH-CH ₂ -O-CH ₂ -NH-CO-R' + CH ₃ OH.

Another class of aliphatic amide derivatives, those with methylated methylohnelamines

can be implemented on the fiber includes compounds of the following general formula:

HO - (CR ² RVNH -COR ',

wherein R ² and R ^{3 are} hydrogen or alkyl groups and η is an integer which is greater than ι. These compounds are easily prepared by reacting an alkylolamine with a higher fatty acid to form the corresponding amide. For example, ethanolamine or propanolamine form amides of the following formula when heated with stearic acid:

HO (CH ₂ ^ -NH-CO-

^X 37

in which n - 2 or 3. These amides are condensed with methylated methylolmelamine on textile fibers in the presence of an acidic catalyst, presumably according to the following equation:

M-NH-CH ₂ O • CH ₃ + HO (CH ₂ ) ,, -NH-CO -> M - NH-CH ₂ -O (CH ₂ ) ^ - NH-CO

'C ₁₈ H ₃₇ CH ₃ OH

From all of this it can be seen that the nitrogen-containing compounds used condense with methylated methylolmelamine with elimination of methyl alcohol. The primary condensation products can be illustrated using the following general formula:

X O

M -NH-GNCR,
where G is the groups

-CH ₂ - and -CH ₂ O- (CR ² R ³ ) _TC -

means, while R ² and R ^{3 are} hydrogen or alkyl radicals, η is a small integer and M, X and R are as defined above.

In these condensation products, at least one of the short-linked groups is methylated Methylolamine replaced by a group which has one or more long in X or R or in both Contains chains with hydrophobic alkyl groups. It should also be noted that the products are also in the melamine core have at least one methoxymethyl group which split off methanol at the treatment temperature capable, with a molecular rearrangement with subsequent polymerization with other alkylated Methylolmelamine molecules takes place. The amido compound, which is the long-linked alkyl group which replaces the short-linked alkyl group, is not cleaved at the treatment temperature, and the long-linked alkyl group remains as a component of the resin, its hydrophobic Evoking properties.

Of course, the subject matter of the invention is not intended to apply to the methylated compounds mentioned Methylolmelamines should be restricted. Other alkylated methylolmelamines can also be used, containing short alkyl groups of not more than 4 carbon atoms, such as e.g. B. ethylated, isopropylated and butylated methylol melamines, although greater care has been taken in these cases must become. The elimination of ethyl alcohol and butyl alcohol during the treatment process takes place less easily in these cases, and also the appropriate heat treatment is more difficult because one must not work at temperatures that damage the tissue.

The alkylated methylolmelamines used according to the invention are made according to known methods Methods shown. So you can, for example, methylated methylolamine by reacting 2 to 6 moles of formaldehyde with 1 mole of melamine to form a condensation product which is predominantly Appears to be methylolmelamine. Under the term methylated methylolmelamine all those reaction products should be understood which 2 to 6 methylated Methylolgrappen each Molecule included. Too extensive polymerization should be avoided during production, since the resin used according to the invention expediently in the form of an aqueous dispersion or solution and products that have been polymerized too strongly are too sparingly soluble in water. It was also found that excessive polymerisation of the product gives the treated fabric a hard feel.

Among the large number of nitrogen-containing compounds that are eligible for the process come, are as preferred representatives z. B. to mention the amides of monocarboxylic acids, which of the following Formula correspond to:

X O

1 I!

H-N-C-R

where X is hydrogen and R is an alkyl radical of at least 7 carbon atoms, such as. B. caprylamide, Capramide, lauramide, myristamide, palmitamide, stearamide, di-n-octylacetamide, oleic acid amide, linoleic acid amide and Rizinussäureamid mean. Other amides of the same general formula can also be used can be used, in which case X also denotes an alkyl group. Such connections are for example N-methyl stearamide, N-ethyl stearamide, N-ethyl lauramide, N-isopropyl stearamide, N-2-ethylhexyl stearamide etc. In addition, amides of the above general formula in which H is replaced by an alkylol group, e.g. B-methylol stearamide, methylol lauramide, ethanol stearamide and further representatives of this class.

Compounds of the general formula can also be used

XO

H-N-C-R

use, in which X is a cyano radical, so z. B. Lauroylcyanamid, Stearoylcyanamid or one Alkylenitrile radical (—CR'RC = N) or when used

of connections, such as B. Di- (octyl) -cyanacetamide, Di- (lauryl) -cyanacetamide, di- (stearyl) -cyanacetamid, N-jS-CyanäÜiyüauramid etc., or a carbamyl radical, as in the case of stearoylurea, or thiocarbanryl residues, for example when using N-myristylthiourea, or a substituted one Carbamyl residue

~ c — n:

wherein R ^{4 is} an alkyl or aryl radical, so for. B. when using N-methylol-N'-stearoyl-N'-ethylurea and N-methylol-N'-lauroyl-N'-äthyUiarnstoff. X can also mean an aryl or alkaryl radical, for example when using stearanilide, stearotoluidide, stearoxylidide and N-benzylstearamide and similar compounds with alkylated methylolmelamine.

It is not necessary that R be an aliphatic radical of at least 7 carbon atoms, provided that the long-limbed, hydrophobic alkyl group in the Veras bond is elsewhere. So is z. B. in connections, such as N-acetyltetradecylamine, R a lower alkyl group and X a long-linked alkyl radical. Other acidic amides of this type can also be used, for example N-acetyloctadecylamine, N-acetyldodecyl arm, N ^ acetyl-2-ethylhexylamine and other connections of a similar character. In addition to these compounds, urethanes reacted with good success as nitrogen-containing compounds with alkylated methylolmelamines will. These compounds are esters of carbamic acid and have the general formula

HO

H-N-C-R

in which R is an alkoxy radical with at least 7 carbon atoms. As examples of urethanes, which can be used according to the invention, may be mentioned octyl carbamate, decyl carbamate, dodecyl carbamate, Tetradecyl carbamate, hexyl decyl carbamate, octadecyl carbamate, etc. Substituted urethanes such as N-methyl octadecyl carbamate, N-methyloctadecyl carbamate, N-methylol dodecyl carbamate and N-ethanol octadecyl carbamate, also give very good results.

In addition to the compounds mentioned, numerous compounds of other types can also be used in the compounds according to the invention Preparations used in conjunction with alkylated methylolmelamines.

There may be, for example, lauroyl dicyandiamide and stearoyl dicyandiamide, in which cases X of the above general formula a Cyanoguanylrest

NH

_c_NH-CN

means called. Compounds such as N-methylstearamide acetate, in which X is a methoxyaeetyl radical ί ° V-

V-CH ₂ OCCH ₈ /

can also be used. When using alkyl esters of nitrocarbamic acid, such as B. octyl nitrocarbamate, decyl nitrocarbamate, dodecyl nitrocarbamate, octadecyl nitrocarbamate, etc., X in the general formula denotes a nitro group and R denotes an alkoxy group.

Mono- and diacyl-substituted ammelines and melamines, e.g. Dioctanoylammelin, Düauroylammelin, Monostearoylammelin, monolauroylmelamine, etc., can also be mixed with alkylated methylohnelamine be used. Compounds of this class have the above general formula in which X represents a heterocyclic triazine residue. In the case of N-cyclohexyl stearamide, X is a cycloaliphatic Rest.

Although most of the above compounds are considered amides of monocarboxylic acids can be, the invention is nevertheless not to be limited to these compounds, since apart from the same also compounds such as di- (octyl) -oxamide, di- (octyl) -succinamide, di- (dodecyl) -succinamide, Di- (tetradecyl) -succinamide, di- (octadecyl) -su'ccinamide, di- (octadecyl) -adipamide, di- (octadecyl) -pimelamide, Di- (octadecyl) -suberamide and di- (octadecyl) -sebacamide etc. can be used in which both substituents may be present on the same nitrogen atom or in which each nitrogen atom can carry a substituent. Other suitable compounds, which are also available as derivatives from polycarboxylic acids include the succinamic acid esters, e.g. B. the Dodecyl ester of succinamic acid, octadecyl ester of succinamic acid, the octadecyl ester of adipamide ioo acid, etc. amides of cycloalkyl, aryl and aralkyl carboxylic acids, z. B. Cyclohexylacetic acid, benzoic acid and phenylacetic acid, which have a long-limbed, Carrying hydrophobic alkyl radicals can also be used. You can also use the Use are N-acylated and N-carboxylated urethanes, such as N-lauroylethyl urethane and N-carbethoxy lauryl urethane, ethyl N-lauroyl carbamate and lauryl N-carbethoxycarbamate.

In considering the various types of connections described above, let us find out that every connection is under the general formula

X O

I Il
Y_N —C —R

falls in which Y is hydrogen or a methylol radical, X is a nonfunctional radical, e.g. B. hydrogen, Alkyl, alkylol, cyano, alkyl nitrile, carbamyl, substituted carbamyl, thiocarbamyl, aryl, cyanoguanyl, Alkoxyacetyl, nitro, a heterocyclic, cycloaliphatic Radical or a carbalkoxy radical, etc. and R represents an alkyl, alkoxy, cycloalkyl, aryl or aralkyl radical mean.

In addition, many other connections can be made according to the invention to apply because how

Mentioned at the beginning, the invention includes those compounds which have an alkyl radical of at least Carry 7 carbon atoms and contain ι nitrogen atom, on which an acidic group and one reactive component consisting of hydrogen or lower alkylol radicals hang. as such compounds not yet mentioned are, for example, methyl-N-tetradecylmethylsulfonamide, N-tetradecylphenylsulfonamide, p-lauroylphenylsulfonamide, N-p-lauramidophenylsulfonamide, etc. enumerated. In these compounds, others are acidic Groups than the carbonyl group

U-)

to activate the hydrogen or the methylol residue, which is attached to the amido nitrogen, effective.

Although it was stated above that at least 1 mole of the amido compound is with 1 mole of the converts alkylated methylolmelamine to form resins of a hydrophobic nature, it was found that it is not necessary to have such a high percentage of higher aliphatic amido compound to be used in order to obtain satisfactory water-repellent properties. In general it has been found that the water repellant properties of the treated fabrics are not essential be improved if more than 5 parts of the amido compound for every 10 parts by weight of the alkylated Methylolamine fall. Usually one becomes approximately 1.5 parts by weight of the higher aliphatic Amido compound per 10 parts by weight of the methylated methylolmelamine in the inventive

Use finishing preparations. However, smaller amounts of these amido compounds can also be used Apply, however, a reduction in the water-repellent properties of the treated Tissue is recorded. Half part by weight of the amido compound for every 10 parts by weight of alkylated Methylolmelamine results in a ratio which textile fabrics are water-repellent in most cases able to do. The advantages of shrinkage resistance, wrinkle resistance, des improved handle, etc. which are obtained with methylated methylolmelamine alone are the Tissues treated by the method according to the invention also own, regardless of whether the Amount of the higher aliphatic amido compound in the treatment mixture is larger or smaller. The inventive, in a treatment of tissues with alkylated methylolmelamine and higher aliphatic amido compounds existing process is expediently practiced so that the treatment solution in the form of an aqueous dispersion which is between approximately 2 to 15% and more of the above materials to which tissue is applied. Such dispersions can be simple by stirring in a suitable amount of the

in a solvent such as B. ethyl alcohol, isopropyl alcohol, Alkyl ethers of ethylene glycol, etc., dissolved amido compound in an aqueous dispersion of the alkylated methylolmelamine are obtained, it being advantageous that both solutions temperatures from 26 to 60 °. If the material to be dispersed is normally a liquid, then so the same is expediently cooled. If desired, each component can have dispersants such as z. B. Sodium isopropylnaphthalene sulfonate, dioctyl sodium sulfosuccinate, N-octadecyl disodium sulfosuccinamine, Add ammonium caseinate, gelatin, glue, gum arabic, etc.

The dispersions can be applied to the fabric in various ways known to the person skilled in the art will. So z. B. immersed the dried fabric to be treated in the resin dispersion and be carried out between suitable rollers in order to effect an even impregnation and eliminate excess solution. The impregnation can also be done by other methods than by Spraying done.

The amount of the treatment dispersion which is applied to the fabric can vary widely depending on the nature of the fabric to be treated, as well as depending on the desired end use. It is possible to make fabrics made of wool, silk, rayon, cotton, etc. water-repellent and also to make these fabrics resistant to shrinkage by applying about 2 to 8 percent by weight of the resin-forming components, calculated on the dry weight of the fabric . It can also contain minor amounts / ₀ reach up to 0.5 ° on the application, however, is achieved slightly less good results. Larger amounts, e.g. B. 8 to 14 percent by weight of the fabric, increase the water-repellent properties of the fabric and also give the same a very high crease resistance. For certain types of fabrics and to achieve certain results it may be desirable to use larger amounts of the treatment mixture, up to 30% by weight of the mixture of alkylated methylolmelamine + higher aliphatic amido compound, calculated by weight, in the mixture. After the fabric is impregnated, it is dried and heated to elevated temperatures to polymerize the resin.

In order to accelerate the heat treatment, the aqueous treatment solution can be given suitable, known per se Add catalysts. Oxalic acid and diammonium hydrophthalate are particularly suitable for this purpose and methyl pyrophosphate, also triethanol aminophosphate, acetic acid, mineral acid, such as sulphurous acid and the like

The curing temperatures are generally low and can vary from approximately 93 to 149 ° with a corresponding reduction in the treatment time at elevated temperature. Both drying and curing can vary widely depending on the equipment available. High temperatures in the range from 135 to 150 ^° will convert the resin into the water-insoluble state within 3 to 4 minutes. In cases where the possibility of treating the resin on the

ewebe does not exist at moderate temperatures in a temperature range of approximately 115 to 135 °,

after impregnating the fabric with the desired amount of treatment solution, the width of the fabric can be removed Stretched on a tenter frame, dried, then roughened on a cylinder and left in the heat until the fabric is completely dry and the resin in the fabric has hardened. at Certain fabrics may require a drying and treatment time of 2 to 3 hours at 93 °. This duration of treatment is in such cases

ίο of course on the effectiveness of the catalyst and depends on the nature of the tissue.

After treating the fabric in the manner described, the same thing occurs, especially in Woolen goods, subjected to a short, tired soaping process to make them soft and pliable. Afterwards can other common finishing treatments, such as decating, brushing, shearing, Ironing, etc. The method according to the invention can be used for colored and for uncolored Goods are used without noticeably affecting the color or shade or the material would be harmed.

The invention will now be explained in detail in the following example, in which the representation of the methylated methylolmelamine, the dispersing ■ method, spray impregnation and the ones achieved quantitative results are described. The invention is not limited to that given in the example Embodiment limited.

example

960 parts by weight of formaldehyde (37 weight percent CH ₂ O) and 252 parts by weight of melamine are introduced into a reaction vessel equipped with a stirrer, thermometer and reflux condenser, which is set up so that it can be evacuated and heated. The contents of the reaction ^{vessel are brought to a temperature of 62 ° within 1} Z ₂ hours and the pn value is adjusted to 7.5 by means of 2N NaOH ". After another half hour of heating, the mixture becomes at a vacuum of about 700 mm of mercury concentrated by removing water. After heating in this way for 40 minutes at approximately 54 °, the vacuum is released and the supply of heat stopped. 1000 parts by weight of methyl alcohol, which _{contain enough 2 nH s} PO _4, are then added.

■ to neutralize the previously added 2 n-NaOH

■ sieren, registered. 'Then the mixture is at a p; a value of 6.4 heated, a mixture of methanol and water being distilled off and one constantly anhydrous methanol is added to replace the distillate. The mixture is then heated for about 6 to 7 hours. Finally it becomes in a vacuum at about 700 mm of mercury to a content of about 80% solids concentrated.

25 parts of the aforementioned 8o ° / ₀ solution of methylated methylol melamine, 20 parts of a 5 ° / _o solution of Natriumisopropymaphthalinsulfonat and 135 parts of water are mixed and heated to approximately 43 °. Then 3 parts by weight of methylol stearariiid are dissolved in 60 parts by weight of ethyl alcohol and the ·. Pour solution at about 43 ^° with stirring into the methylated methylolmelamine solution. A constant fine dispersion is created. This will eventually Diammoniumhydrophosphat added in an amount of from 4 ° / ₀ calculated on the weight of the resin. Samples of cotton fabric (Perkai) with a thread count of 31.5 threads per centimeter in the warp and in the weft were impregnated with the dispersion described by the immersion process by dipping the fabric in this dispersion of the mixture and squeezing off the excess by means of rollers and if necessary repeated the process until the desired amount of the preparation was absorbed. Assume that the dispersion used contained 11.5 percent by weight of the mixture and the wet pick-up was 100 ° / _0, the amount of solid, methylated methylol methylol + was about 11.5 weight percent of the dry fabric. In this weight, the removal, and then drying the impregnated fabric at 144 for 7 minutes was carried out ^0. Then was a short soaps by treated to ^x / ₂ hour at about 70 ⁰ in an o, 5 ° / ₀ soap solution, followed rinsed and dried. Other samples of the treated fabric was soaped in an o, 5% soap solution for 4 or 6 hours at about 70 ⁰ to the water-repellent effect of the treated tissue observed. Still other samples were cleaned in a Stoddard solvent at room temperature for 2 and 4 hours to test the resistance of the finish to dry cleaning. All samples were then tested for water-repellent properties using a normalized test method as follows:

A square section of fabric with a side length of 15.24 cm was ^{hung at a distance of 25.4 cm from a horizontal spray nozzle which was pressed with water of about 26 °} under a pressure of 1.83 m water column. The section was sprayed for 1 minute during which 5.7 liters of water flowed through the spray nozzle. The fabric sample was then allowed to drain for 10 seconds, rolled between pieces of absorbent paper to remove the water adhering to the surface and weighed. The weight gain due to the absorbed water was expressed as a percentage of the original dry weight of the fabric. An untreated swatch of fabric thus absorbed about 90 to 100% of its own weight in water.

A large number of long-limbed, alkyl-substituted Amido compounds were dispersed with methylated 1x5 methylolmelamine and in the manner described above Way brought to the tissues. While the absolute results varied to some extent, it could at least be determined that in each case the fabric is extremely water-repellent was. It has also been found that other dispersion methods can also be used and that the water-repellent effect increases with the smallness of the dispersed particles.

Methylol dodecyl carbamate was treated with methylated methylol melamine by dissolving the former in the five

times the weight of ethyl alcohol and by pouring this solution into a dispersion of methylated methylolmelamine, as described above, dispersed. Dodecyl carbamate was similarly dispersed with methylated methylol melamine and applied to tissue. Methylol stearoylurea is a very insoluble material so that it is more difficult to disperse. When working with this compound, it was necessary, 70 parts (by weight) ethylene glycol monoethyl ether for dissolving 3 parts by weight to about 82 Methylolstearoylharnstoff apply ⁰ when heated. The results obtained with dispersions of this compound and the results obtained with other compounds are shown in the table below.

Spray test at 80 ° moisture absorption in percent

at 70 °
1 in o, 5 ° / ₀ sodium soap
soaped solution 28 dry cleaned in
Stoddard Solvent
at room temperature 4 hours 39 30 min. 4 hours 6 hours 2 hours 1.5 parts methylol stearamide 28 37 28 (30 minutes) + 10 parts of methylated methylol melamine 27 29 28 1.5 parts methylol dodecyl carbamate - 33 24 (30 minutes) + 10 parts of methylated methylol melamine 27 29 26th 1.5 parts of dodecyl carbamate 47 29 (30 minutes) + 10 parts of methylated methylol melamine 27 28 1.5 parts methylol stearoylurea - 36 - (- 10 parts of methylated methylolmelamine 33 46 1.5 parts of N-acetyltetradecylamine - + 10 parts of methylated methylol melamine 28 27 ' 1.5 parts of stearoylcyanamide + 10 parts of methylated methylol melamine 24 28

The results of these spray tests show that the samples are very hydrophobic. The water repellent Properties are retained both after normal washing and after a dry cleaning process obtain. In addition, it was found that the shrinkage caused by washing the fabric sections are very small.

The dispersible mixtures which can be used according to the invention can also be prepared by methods which require fewer solvents and less expenditure of time. So were z. B. 50 parts by weight of crude stearamide, 90 parts by weight of 95 ° / _o strength ethyl alcohol and 17 parts by weight of a registered io ° / ₀ solution of sodium dioctyl sulfosuccinate in a vessel equipped with a stirrer, a reflux condenser and a thermometer, the reaction vessel. This mixture was heated to reflux for so long was solved until everything stearamide, and then cooled to 70 ^0th Then, this reaction mixture was admixed with 6.2 parts by weight of 30 ° / _O igeni sodium hydroxide dissolved in 23.2 parts by weight of 37% formaldehyde igein. The contents of the reaction vessel was maintained for 1 hour to 70 to 75 ^0th Then a mixture of 414 parts by weight of 8o ° / ₀ sodium methylated methylol in methanol, 17 parts by weight was added to the hot reaction mixture was added a solution of sodium dioctylsulfosuccinate io% and 34 parts by weight of water in the tank. This created a paste-like mass, which was vigorously stirred to ensure complete mixing. The paste was then passed through a homogenizer to obtain a uniform consistency. Such a product is nice

therefore particularly suitable because it can be easily stored and shipped. The same thing just needs with To be diluted with water and treated with a catalyst to create a dispersion of fine grain size, which is suitable for impregnating fabrics.

A similar product was prepared as follows: 50 parts by weight of crude stearamide and 90 parts by weight of denatured alcohol were added to a reaction vessel and heated to about 80 °, a clear solution being formed. After cooling the solution 8o _^0/0 sodium methylated methylol in methanol was added to 414 parts by weight. Then at 5 immediately 20 parts by weight of a 37% formaldehyde solution and 5.2 parts by weight of 37% sodium hydroxide were added to the reaction mixture. The temperature was then slowly raised to 75 ^0, at which temperature a clear solution, it was heated for a further I ¹ Z ₄ hours at 70 to 75 ^0th After this treatment time, the temperature was increased to 78 ° in order to clarify the solution. Finally the solution was poured into a reaction vessel and slowly cooled.

Aqueous, for the impregnation of fabrics suitable dispersions were obtained by mixing 72 parts of the paste described above with 72 parts by weight of water and 20 parts by weight of io ° / ₀ solution of sodium isopropylnaphthalenesulfonate. This mixture was heated to boiling and the clear solution was then again diluted with 226 parts by weight of water with rapid stirring. To this dispersion were added 20 parts by weight of io ° / ₀ solution of Diammoniumhydrophosphat added. Tree-

pieces of wool with a thread count of 31.5 threads each

per centimeter in the warp and in the weft were then impregnated with this mixture. The so treated and rinsed test pieces showed the same good water-repellent properties, as indicated in the table below.

Carboctadecoxycyanamide, octadecylcarbamate, methylolooctadecylcarbamate, stearoylcyanamide, diacetyldecanoguanamine, N-myristoylthiourea, lauroylcyanamide, stearoylurea, methylolauramide were ίο also dried in the manner described above, treated with methylated methylolmelamine and dispersed in the heat, the fabric was also treated with methylated methylolmelamine and applied in the manner described above. After the soaps at about 70 ⁰ in an o, 5 ° / ₀ soap solution for 30 minutes, this fabric had water-repelling properties on the order of those compounds which were cited in the surrounding table. Even after soaking for 4 hours and after dry cleaning and soaking for 30 minutes, these fabrics retained their water-repellent properties.

Below that mentioned in the description above

Stoddard solvent is one at about 150 to 120 ° boiling petroleum hydrocarbon fraction to be understood (see British patent specification 555 480, p. 2, Lines 71 to 74).

Claims (8)

PATENT CLAIMS: i. Preparation for finishing, especially for Making textiles water-repellent, characterized in that they are essential components contains: a) an aqueous dispersion of one with Alcohol-converted methylolmelamine of the form that etherifies at least two methylol groups are, the alcohol with which the methylol groups have been reacted, has no more than 4 carbon atoms in the molecule, and b) a compound of the general formula containing a nitrogen atom X O Y_N - C - R in which Y is hydrogen or an alkylol group, X and R are hydrogen or non-reacting substituents or alkyl groups with at least 7 carbon atoms, with at least one such alkyl group is present and the compound in the dispersion in an amount of 0.5 to 5 parts by weight for every 10 parts by weight of the Methylolmelamine is present. 2. Preparation according to claim 1, characterized in that that the compound (b) is an amide of an aliphatic monocarboxylic acid with at least There are 8 carbon atoms in the molecule. 3. Preparation according to claim 1 and 2, characterized in that the compound (b) is a stearamide, Is methylol stearamide, ethylol stearamide or methylol lauramide. 4. Preparation according to claim 1 to 3, characterized characterized in that the compound (b) in an amount of about 1.5 parts by weight for every 10 parts by weight of methylolmelamine is present. 5. Preparation according to claim 1 to 4, characterized characterized in that it contains 2 to 15% of the components a) and b). 6. A method for finishing a textile fabric, characterized in that the fabric treated with a preparation according to claim 1 to 5 and then to insolubilize the Harzbüdenden constituents of the treatment agent is heated. . 7. The method according to claim 6, characterized in that the treated fabric is heated ^{to a temperature between 93 and 149 0.} © 5660 1.53