DE1469504A1 - Process for the treatment of textiles with aminoplasts - Google Patents

Description

(US 531,952 - Prio 14. Au _C. 1963

U6950A

West Point Manufacturing Company West_loint, Georgia, V.St.A.

Dr. Expl.

Hamburg

, July 27th

de »« «narrowed

W.derat.nd.fability against »« «« -1— IL u. D.r Obermoe an an- .res M ^ - - - ·

_e to WU. - * - *

009831/1760

Catfish take place; ; aeist but is cured in the presence of acidic, catalytically v / irkenden substances bsi temperature of 150 ⁰ and höhar. In the case of the urea-foiiraldehyde-amino loads, the impregnated textiles were sometimes only dried in the presence of an aromatic substance. The hardening is dos treated after a 12nge3? S retention substance ", for example by JO days cöav more complete. In another hardening process with aminoplasts Hir-d worked on a wet way, either for a long time at room temperature or at a slightly elevated temperature.

Most treated textiles, however, are usually cured at higher temperatures; this also applies to the egg-soldering of aminoplasts. In many cases, the high working speed requires short curing times, which enables a more precise control of the properties of the textiles treated. However, there are some disadvantages here, in particular a loss of strength properties such as tear strength, tensile strength and abrasion resistance; Furthermore, the suppleness and suppleness of the tissue suffers, although this can in part be restored by the application of softening agents and other substances.

When hardening over longer tent spaces, one generally obtains worse qualities; the strength and others

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Elgenaohaften also never suffer from hardening at high levels Temperatures, in addition to which the folds or creases in the fabric treated in this way are usually fixed will.

Hardening according to the wet method, as for example in accordance with ÜSA patent application 2 76? 57 ^ is described Primarily used to fix polymeric melara compounds in or on cellulose textiles. With this one Processes, for example, require light impregnated textiles for at least 8 minutes and heavier fabrics even longer exposed to steam treatment. Curing is usually done in batches. The material is used e.g. on orphans rolled up and damp for at least one or more days held. This must prevent drying out »ferden, e.g. by wrapping the rolled up balls in waterproof material. If the fabric before the wet curing dries, the possibility that dry cure will occur increases. You can also work continuously, if special systems are used to ensure even steam treatment of the substance for very long periods of time; you can also use a usual Damping system work, however, the Le & ung is considerably reduced. However, this is for economic reasons Reasons not acceptable, since the discharge can generally be reduced by a factor of at least 10 or more

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nut; (For example, the normal dwell tent in a dye steamer with slightly heavy textiles cheats JO seconds; increasing the dwell time to 10 minutes reduces the dwell time of the steamer by a factor of 20.) For these reasons, continuous treatment of the fabric using the wet process at high speeds is possible general impossible. If this wet process is carried out carefully, the physical strength properties are not affected as much as with dry curing, although some stiffening of the fabrics occurs.

The present invention aims at the various Eliminated disadvantages and suggested a hardening process in which the long hardening by the wet method or the dry hardening at high temperatures is no longer necessary, and which is continuous with a great deal of impact on the usual Attachments can be carried out. If done carefully, the strength properties become little or not influenced at all «and no stiffening of the fabric as with dry curing is observed. The treated textiles are sniff-resistant and do not rot and are crease-resistant. These and other purposes are achieved through the use of a hardening agent or a catalyst which is quite a Syriac English combination

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contains certain components, namely an acid and a sour salt. The aminoplast is made from an aqueous Solution or dispersion applied to the fabric, and the Catalyst is fed either with the dispersion or completely or partially after the aminoplast. the Impregnated textiles, for example, are heated with steam while they are still moist and can then be washed and dried. The hardening can also be carried out in such a way that the material: only at slightly elevated temperatures, e.g. of 120 ° or less, dries, whereby Care must be taken that the material is not excessively heated, surprisingly it was found that the extremely active catalysts accelerate the hardening of the aminoplasts during steaming or drying at moderate temperatures, but that they do not the stability of the solutions or dispersions of the aminoplasts at room temperature or slightly elevated temperature interfere significantly or no longer interfere than the catalyst systems previously used in wet curing.

The aminoplasts used in accordance with the invention comprise reaction products of nitrogenous bases with aldehydes, which are either soluble in water or diapergatable in water. Typical nitrogenous bases are. Melamine, Ouanamlne and other triazines, urea, ethylene urea,

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Propylene urea, thiourea, guanidine, biuret, dicyandial, uron and numerous derivatives thereof, as well as cyclic imines and xthylenin and propylenin. The aldehydes belong to the group of compounds which form water-soluble or water-soluble condensation products with nitrogenous bases, although formaldehyde is preferred. The aminoplasts can be completely or partially etherified with methyl or ethyl alcohol or other higher alcohols. It can also be a mixture? from aminoplasts can be used. Finally, combinations of aminoplasts with numerous modifying agents such as water-repellent agents, substances for refractory treatment, softening oils, stains and paints can be used, provided that these do not interfere with the reaction with the aminoplasts. The aminoplasts can react in such a way that they form repeating units or that they react with other substances such as hydroxyl groups, nitrogen-containing radicals, thio or oxyran radicals. It has been found that compounds containing these residues can give a secondary synergistic effect. For example, fixed _/ epoxydlerte that provides triglycerides was, cause a significantly higher fixation of aminoplasts in and on the fiber surface.

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The hardeners contain an acidic component and a Salt. The acidic component can be one or more Bono, dl or polybasic acids, namely organic or mineral acids, which in the case of the primary acids are not so much more acidic than acetic acid or which, in other words, have a dissolution constant at room temperature which is not less than 10. Suitable acids include formic acid, sulfamic acid, Olicolic acid, oxalic acid, citric acid, diglycolic acid, tartaric acid, sulfurous acid and orthophosphoric acid. These acids are preferred because they are inexpensive, readily available, easy to use, and the like, but auoh other acids from this range can be used. Formic acid is particularly suitable.

An Aranoniura salt, an AmIn or a is used as the salt component Metallealζ an organic or inorganic acid used, which in an aqueous medium at room temperature or an increased temperature reacts acidic. This also includes combinations of salts that do not have any in the isolated state show acidic reaction, but in combination with other salts do not change the properties of the combination in such a way that one acidic reaction at room temperature or at elevated temperatures ▼ is reduced. Examples of catfish can be the ammonium * Amine and metal salts of hydrochloric acid and other halogen

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acids, sulfuric acid, thiosulfuric acid, the other acid, sulphate acid, phosphoric acid, phosphorous acid, fluoroboric acid, nitric acid, nitrous acid, carboxylic acid, and sulfonic acids are used either alone or in combination will. For example, because of their low cost and easy availability, amonium sulphate, ammonium sulphate, Aaeonium sulfite, Aisaonium bisulfit, An & oniuathlosulfat, Anvmlundihydrogenphosphat, Dlanmoniuaphosphat, Amnonlunsulfamat "Anaoniuianitrat", Aneonlumecetat, Aanoniumitrrat " 2-aninopropanol hydrochloride, magnesium chloride, magnesium sulfate, magnesium sulfate, AlumlnluBiehlorld, AiuinluBacetat, AlUBinlutisulfat, Zinc chloride, Zinc acetate, Zinc nitrate, zinc fluoroborate, calcium chloride, barlunchloride, perrichloride, stannic chloride and chromium chloride are used will. This shows that a large variety of salts in the processes according to the invention have an advantage can be used. However, magnesium chloride is particularly preferred.

Textiles made from natural ones can be used as textiles and regenerated cellulose fibers or made of fiber materials with other fibers, synthetic fibers and mixtures with other fibers such as polyamides, polyesters, polyolefins, acrylic acid fibers or other synthetic fibers are used are made from animal fibers, all of which are solid

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and vegetable fibers, where the fibers can occur naturally or are made from non-colored components will.

All textile products for which the main body consists of a flat material consisting of threads, namely woven ©, knitted, non-woven and similarly composed textiles, yarns, PJtden and fihnliohe paser formations »which are either spun, are twisted, twisted or pretreated for other catfish such as threads, rovings and other paser arrangements lying next to one another in an ordered or disordered or heaped arrangement. It also includes paper and others Paper products made from natural or synthetic fibrous materials.

The catalyst amounts range from 0.1 to 4 % acid and from about 0.1-4% salt, based on the weight of the solution, although concentrations outside this range in some pills may also be suitable. Usually the acid and salt are used, however, in amounts of 0.5 to 1.5% by weight.

To carry out the treatment, the textile material is first subjected to an aqueous reading or suspension of the AsdLno Plastics and the catalyst ispHMpUert, either

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In a single bath or in several baths. Impregnation can be done by dipping and the like. In general, however, the aminoplast and the catalyst are applied from a single bath which is at room temperature or a somewhat elevated temperature, but usually at no more than 30 ° C. The uptake of aminoplast is usually around 1 -> 15 Jtf, based on the dry weight; However, larger quantities can also be taken in special volumes. Under certain conditions it is advantageous to apply the aminoplast from one bath and the catalyst from another. Such a separation of the components results in a longer service life of the bath with the aminoplast and allows higher working temperatures during impregnation. The maximum temperature in the aminoplast depends primarily on the heat resistance of the aminoplast used; with some aminoplasts, and especially with those that do not form insoluble residues in non-catalyzed solutions, practically all working temperatures can be used. For the catalyst solution, the temperature is usually 82 ° or higher; However, practically any temperature γόη room temperature up to the boiling point can be used. After application of the aminoplast and catalyst, the treated textile material is hardened in one of the following three ways: · J

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1. The treated textile material can take about 15 seconds or less subject to steam treatment for up to 5 minutes. If oars or fibers lh one Heap are treated, the steam side can be increased so that the entire mass is actually subjected to a steam treatment. In general, the However, the fixing temperature for common fabrics is about 15 to 90 seconds and usually 30 to 60 seconds Seconds, wherein the steam temperature can be 100 ° or more and in particular 105 to 120 °.

2. The treated textile material can simply be dried to induce hardening. Preferably white the dry temperature is in the range of 105 to 120 ° C although temperatures outside of this Berelohes can be used. The main point of view is that the treated textile material does not heated over a temperature range of 120 to 150 ° otherwise the tissue will be damaged or destroyed. Time and temperature of drying depend on the relevant conditions of the plant and the textiles to be treated.

J. The treated textile material can be hardened by leaving it in a moist state. Although one of the main advantages of the invention

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Process lies in the fact that the process can be carried out at high speed and continuously, it can be more advantageous in some grooves to treat the textiles intermittently. In such pills the curing takes place in a period of only 2 hours at 32 to 38 ° C ₄ although the treatment can be extended without damaging the textile material. You can also choose to reduce the treatment time by increasing the temperature during this treatment or storage tent.

After curing, the textiles -with water, optionally aiii washed with a surfactant or other washing aid and dried. It is also possible to have a to perform wet fixation with a dry hardening. In this way, the properties that occur as a result of wet fixing are strengthened, and if strictly observed the working conditions have little or no harmful effects. The treated textile material can therefore can simply be dried at a higher temperature without washing after the wet fixing in order to achieve an improvement in properties in general. You can also choose to wash the textile material after it has been wet-fixed, see what the application of the usual hardener accelerators or catalysts such as ammonium amine, magnesium, aluminum and Zinc salts of hydrochloric acid, phosphoric acid, sulfuric acid,

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Nitric acid »fluoroboreic acid and other acids or one Stubborn look at it. DIb damage to the dry to prevent or reduce hardened material « the textile material in general only as indicated above after application of the dry hardener dried » although the temperatures and drying times can be as high or as long as possible as such Tea rooms and tents are desired »the textiles that are to be treated with the appropriate treatment and su- ' are suitable.

I am a surprising feature of the method according to the invention ", in which] the textile material is not only in contact for a short time after the treatment solution, such as in immersion baths or tubs, etc., consists in »that the bar crops up on the textile material to be treated. This makes it possible to use the textiles in a vernal, tnl nmMsslg low «concentration Treat aminoplast see below and a high concentration of fixed aminoplast on the treated textile material see below achieve. Venn, for example, the same oarns in a tub

'Γ I

with a catalyzed solution with a · content of 4.2 % ■

■ I. Γ

Aminoplast were treated and working sows

Except for the temperature of the treatment solution were the same » The average fixation of aminoplast at working temperatures Ie was from 27 to 4 ° Ot

QQIIIt

Fixed aminoplast temperature

27 ° C 5 * 2 %

38 ° C 7.6 %

* 9 ° C 9.9 %

In the same way, the spring tent affects this Exhausted the horse's exhaustion, so do others Factors like s.B. the particular catalyst combination used, the aminoplast and the type of pretreatment of the textile material ». .,

The cracking rarities and temperatures are only through determines the stability of the treatment solution concerned. That brings that the tent and temperature of the EraohCimp in such a way as to prevent precipitation or coagulation of the remaining aninoplasts in the air does not occur.

Instead of the steam treatment, according to another embodiment of the inventive kissing process, the padded textile material can consist of the amino

plastlusung or -dispersion ndt or without slure or sale by a solution of a salt «of an acid or by a Solution of a Salses and an SSure, which to an elevated temperature and preferably to 82 ° and holier is held. B. in a further execution foni de «

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The process of the invention becomes a non-catalyzed one Aminoplast solution, or an aminoplast solution, which is a Component of the acid / salt catalyst solution either helss or cold contains "applied to a textile material, followed by the catalyst system" or the second Component of the catalyst system hot or cold on the Textile material is applied, which can then optionally be fixed by steam treatment.

Bs a simple method was developed to advance the catalyst system for the wet fixation of aminoplasts to estimate. Here, a measured amount of a Solution or dispersion of the aminoplast, which contains the relevant catalyst to be examined, in a Given a test tube, which is in a water bath of a thermostat of 82 ° C. The condensation of the Aminoplasts required tent, which is recognizable by a cloud formation or precipitation, is determined at the temperature at which such cloud formation or precipitation occurs; this is a measure of the catalytic efficiency of the system to be examined. In this way, for example, the relative Determined effectiveness of various chlorides in wet fixation. A standard solution was used in this series of experiments of a methylated melamine resin with formic acid or at the same concentration in other containers

009831/1780 " ^l6 "

Formic acid and ammonium chloride or magnesium chloride, Zinc chloride, aluminum chloride and perrichloride or old Hydrochloric acid catalyzed. In these procedures, it was found that the relative rate of reaction of these

l. I.

catalytic systems based on formic acid in the the following order of magnitude:

NH4C1 \ HgCl ₂ \ FeClx ZnCl ₂ N AlCl,>HCOOH> HOl HCOOH r HCOOH * HCOOH ^β HCOOH ' HCOOH

'4

You relative rate of reaction of a salt in However, this system is not necessarily to bring with it the acidic character of the salt. This investigation only applies to those aminoplasts which form insoluble polymers. Bs will however attempt with this one a good indication of how to select the catalyst systems are »in the case of aminoplasts, which are not insoluble Form polymers.

The invention is to be explained in more detail below with the aid of examples.

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BelBPlel 1

A cotton twill with a surface weight of 298 g each 0.836 in ² was desized, degreased, dyed and durohewasohen, freed of all residues and then continuously passed through a vat, steam and washing chamber. In the vat there was an aqueous solution of

12 pounds of methylollated melamine: 1.0 % magnesium chloride hexahydrate 1.0 % formic acid

0.2 % polyethylene oxide condensation product with nonylphenol (wetting agent)

This solution was at room temperature. The residence time in the steam chamber was 60 seconds. The total corrugated tent in the facility was 2.1 / 2 minutes. The fabric was dried continuously for 2.1 / 2 minutes at 150 ° C.

The shrinkage in the warp and the breaking strength were measured on 1. the treated fabric, 2. the untreated fabric and 3. a fabric treated as above, However, no magnesia urachloride hexahydrate in the now Bath solution was present; aioh resulted in the following Evaluates

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Shrinkage breaking strength

the chain chain weft

In kg / 2.5 ow

1) 6.8 % 64.9. 37.2

2) 20.8 % 63.9 36.3

3) 18.9 % 63.5 36.3

These values clearly show that there is a significant improvement in the response capacity in the chain without a change

the strength of the fabric is achieved. That treated Textile material dried flat and smooth, which was not noticed by the others; the treatment resulted in ' no stiffening of the material.

Example 2

The procedure used was the same as in Example 1, except that a one percent magnesium chloride hexahydrate solution was applied at 180 ° C. during the last washing stage and then dried at 150 ° C. for 2.1 / 2 minutes as before. The shrinkage of the * warp for this fabric was 5.3 % * the breaking strength of the warp or the weft thread was 63.5 or} 6, J) kg / 2.5 cm.

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Example 3

Example 2 similar to the method was used; A fabric was used as the textile material, the threads of which had a core made of polyamide fibers with an outer layer made of cotton. The treated fabric and one corresponding untreated fabric swatches were 45 seconds heat curing under the same conditions at 193 ° C

subject. It was found that the shrinkage of the treated fabric in both weft and warp direction was less than 50 % of the shrinkage of the untreated fabric and that the treated textile material did not yellow during the heat treatment like the untreated fabric. When washing after heat setting, the shrinkage of the treated fabric was much lower than that of the untreated material. The treated fabric could be washed without fraying and dried smoothly and flat, while the untreated fabric severely frayed during washing, dried badly and wrinkled.

Example 4

A terry toweling material was treated according to Example 1. Again it was found that the dimensional stability or dimensional stability of the textile material was not impaired

the strength and without stiffening significantly improved could be. When the treated fabric was washed, the terry loops remained upright and resilient in contrast

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su a similar but untreated washed material that looked flat and compressed. The absorbency of the treated and untreated fabric was examined the absorption capacity with the wick method; the treated material had an absorbency of 91.4 mm, while the untreated material only has one value of 81.3 mm. The absorptive capacity of the treated) So the fabric was slightly higher than that of the untreated.

Example 5

A cotton linen was treated in Example 2, but now the melamine concentration in the treatment bath was 18 % . Much improved dimensional stability and smooth drying properties without loss of strength were observed; furthermore, the fabric retained all of its strength when stored for 2 weeks under damp earth, the composition of which was such that an untreated fabric completely decomposed during the same period of time.

Tests on cotton fabrics that had been treated according to the invention with old melamine-formaldehyde resins showed that 90-100 % of the resin applied was fixed on the fabric. In these experiments, among other things, the material was dissolved in 5 liters of aqueous phosphoric acid with a content of

^ ^{; i /} -21. "009831/1700

boiled from 1.5 % urea until the material responded negatively to phonoaldehyde, which usually took 30 to 60 minutes; the weight loss was then determined. The content of retained resin corresponds to the fixed amount. Comparisons with fabrics that had been treated in the usual way and were wet-cured resulted in a 70 #Lge fixation of the applied resin; in the case of dry curing, about 70 % of the resin applied is also fixed.

Example 6 Meroerlslertes cotton yarn was placed in a tub with the

the following solution:

4.2 % commercial triazine resin (Aerotex resin 23) 0.75 % magnesium chloride hexahydrate 0.75 % formic acid

0.2 % polyethylene oxide condensation product of nonylphenols (surfactant)

The approximately 38 ° warm solution was for 30 minutes through the Yarn headed; Then the excess solution was removed and the material was kept for 3-16 hours at room temperature left and dried. The treated yarn was tested for shrinkage on Trookensijangen; here ! '-22-

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It was found that the yarn treated according to the invention showed no puckers or crimps regardless of the 2 or 16 hour pretreatment before drying, while the untreated yarn creased or puckered heavily in this shrinkage test. A chemical investigation showed that the amount of resin drawn up during the process was practically the same for the different types of yarn, regardless of whether they were aged 3, 4, 5, 6, 7 or 16 hours before drying. The average high resin content was 7.6 Ji. The durability or adhesiveness of the resin was such that more than 90 % of the resin present in the dyed and finished wound yarn was still present after 30 washes.

Example 7

The solution according to Example 6 was applied to untreated or mercerized or bleached and to mercerized and bleached cotton yarn, the solution being 50 ° C. and the saturation time being 50 minutes. Before applying a solution of sodium metabisulfite # 0.5, 0.25% tetrasodium pyrophosphate and 0.1% aqueous _ammonia) was allowed nlak the yarn 3 hours or longer in the wet state. The solution was applied at 82 ° and then dried. This yarn did not show any shrinkage crimp on the drying bars. Furthermore, was

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found »that the hars had stabilized the yarn so thoroughly * that normal bleaching did not remove the normal color of the untreated and the nercerized yarn. The bleached and bleached and bleached oars, on the other hand, did not suffer from discoloration due to processing and could be used in standard white towels because of their degree of whiteness. The absorption or setting of the resin was 10 - 12 % for these oils. After doing 30 household laundry, the treated yarns were found to hold 90% or more of the aminoplast present in the finished product.

Example 8

Merolized and bleached cotton yarn strands (20 * s / 2) were treated for 30 minutes at 30 ° C. in a solution similar to Example 6. The oarn was placed in a moist, impermeable envelope for 28 hours at 66 ° C. and subsequently dried at 104 ° C. The increase in weight showed that 9.7 % of the impregnating agent had been absorbed; this value was determined to be 9t * % by nitrogen analysis.

Large varieties of yarn were treated under identical conditions, but now 1 % of an epoxidized

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Triglyceridee (Epoxol 9-5) was added to the impregnant as an emulsion. The amount absorbed was determined by weight gain to be 18.6 % and by nitrogen analysis to be 13.1%.

This example shows that the aminoplasts are located on the can exhaust treated textile material and also the synergistic effect of the epoxidized triglyceride.

Example 9

A cloth measuring 136 × 64 cm, which had been merged and bleached, was immersed in an aqueous treatment solution of the following composition:

3.3 % triazine resin

0.84 # epoxidized triglyceride 0.5 # zinc fluorate

1.0 % citric acid

0.2 % ethylene oxide condensation product of nonylphenol (wetting agent)

The cloth was treated for 60 minutes at 66 ° , squeezed off to 60% of the absorbed solution and left for 2 hours at 66 ° C in a sealed polyethylene envelope. Then the fabric was dried at 105 °, in alkaline

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Washed with water, rinsed and dried again. The weight increase, based on the untreated fabric, was 11.5 crew. $>.

Example 10

This example only shows that the epoxidized triglyceride is hydrolyzed to some extent in the treatment and acts as an acid component of the catalyst and also as a reactant. The process of Example 9 was repeated, but instead of the citric acid, 0.25 % formaldehyde and 0.5 % acetone were now added to the aqueous system. All other treatment conditions were the same. The weight increase was 17.0 %, based on the untreated material.

Example 11

In a continuous process, an army drift became a challenge or army lines with a basis weight of 255g passed through an aqueous solution containing the following compounds contained:

16.4 % triazine resin

6.1 % emulsified fat derivatives of melamine

Formaldehyde (water repellent)

1.2 % magnesium chloride hexahydrate

1.2 % formic acid

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The fabric was steamed for 1 minute at 105 ° C treated, washed at 60 ° C and passed through a solution of 82 ° C, which 3.7 ß / 1 of magnesium chloride hexahydrate contained. Then the toxin material ran low at 150 ° C dried.

This textile material had a spray value according to AATCC standard test method 22-1961 from ICO and retained its entire strength even after storage for two weeks in a soil in which untreated textile material was completely destroyed in 7 to 9 days. The shrinkage in the chain was ¹ % for the treated material compared to 9.9% for the untreated material. If a container was formed from the cloth, filled it with water and hung up at the corners, no penetration of washer was found after 2 hours, whereas non-bundled material immediately penetrated water in a similar experiment.

This example clearly shows the effectiveness of water repellency in the method according to the invention.

In other attempts it was separate and common Use of the catalyst components investigated. The textile material was impregnated with an arainoplast solution, which the acid component alone, the salt component alone or contained both components together; the fabric was

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then continuously from a vat, which the behend · solution contained, 30-60 seconds through a steam chamber guided and washed afterwards. It was found that essentially the wet fixation only takes place on the substance which is treated with the solution which contains both catalyst components, whereby the synergistic effect becomes clear.

Due to the unique properties that are made impossible by wet drawing or fixing, the most varied of effects can be achieved with all kinds of textiles. For example, the inclination of the canoe i textile on to shrink including washing, in some cases significantly reduced, or by treatment with an aminoplast naoh the present wet Fi ;; c ycle £ sverfehren be eliminated. The tendency of some textiles, and particularly poly aiii de, to shrink during heat setting or heat treatment can be significantly reduced. The textiles can be colored by incorporating suitable dyes and pigments into the resin solution, wzf swcr also such ·? Textiles made of synthetic fibers, wc] are known to be difficult to dye. You can choose to change the color of the textiles, for example by using ferric chloride in the aminoplast solution and then washing with alkaline media

V-V

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Develop fixation, an insoluble colored elsenic compound precipitating and producing the coloring in situ will. Cotton yarns can be fixed by wet: or Pulling up an aminoplast in or on highly twisted Yarns and then turning back the yarn treated in this way convey certain stretching properties. Yarns for the edges of towels or edging tapes, which are much stronger due to the geometric Si; off formation shrink than the usual fabrics and pile yarns, can be made more resistant to shrinkage during washing and do not show the usual warping of the towels due to this shrinkage. The after Fabrics treated with this process, and in particular cellulosic fabrics, exhibit better compliance and flexibility smooth drying properties without stiffening. The treated textiles are opposed to biological degradation resistant. By adding or incorporating other suitable substances into the impregnating agent, the treated textiles can still be waterproof, fire-proof and resistant to Surface changes and lightfast can be made.

The textile material can be stitched, stiffened or opened other catfish are modified to have certain characteristics like the so-called "handle", better sliding on the hem or to achieve better sewability.

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For example, in one embodiment, the present invention with the aminoplast mentioned is the product known as "Phobotex FTC" from the Ciba Company harden, which is a fatty acid derivative of melamine, which is precondensed with melamine and a self-condensation and can carry out conversion with cellulose. This material can be used as a fatty acid-melamine-formaldehyde precondensate be considered which is emulsifiable and when hardening on a fabric made of cellulose or synthetic Fibers created water-repellent properties.

Normally Phobotex FTC and require ähnliehe water repellent agent curing at elevated temperatures of, for example, 150 ⁰ C and higher, with the curing time depending on the curing temperature and, depending on the thermal properties of the water-resistant to making furnish for several minutes

such temperatures. Such dry curing can be detrimental to the fabric. As a result, will With the process according to the invention, a significant advantage is achieved, namely by now being carried out at lower temperatures can harden. This is illustrated by the following example:

Example 12

Stripes of a bleached or an unbleached army cotton drill with a basis weight of 294 g

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- by means of an impregnation solution of the following composition passed through:

Triazine-formaldehyde precondensate - 13 wt% fatty acid MelaminSormaldenyd-.

Precondensate (eraulgiert) - 5 * 5% by weight.

Zinc Pluoborat -1.0% wt.

Formic acid - 1.0 Gev /. %

Alkylphenol-ethylcnoxide condensate

(Wetting agent) - 0.1 Gev /. %

The strips were continuously impregnated with this solution, steamed at about 105 ° C for 60 seconds, and washed with 60 ° C water. The fabric took up about 50-60 % of the impregnation mixture. After washing, the fabric was dried as a continuously moving strip for 3 minutes at 120.degree. The treated fabric had the following water repellent properties:

AATCC AATCC AATCC Break-proof-spray-water-duck-hydrostability (W χ P) value IKsigkeit tischer _{ln k} "

Bleached 100 0 ml 41.2 cm 79 # 3 x drill

Rough drill 100 2.7 32.5 cm 69 χ 66.2

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In a comparison experiment, the zinc fluorate and formic acid from the above impregnation solution were replaced by 2.1 % magnesium chloride. Strips of fabric from the two text materials were passed through the new impregnation mixture and took up about 50 - 60 % ; The strips were then dried at 120 ° for 3 minutes and cured at 164 ° C. for 3 minutes. They were then washed in water at 60.degree. C. and dried again at 120.degree. C. for 3 minutes. The only differences between these two strips of fabric were therefore only the catalysts of the two mixtures and the manner in which they cured. The textile material treated with the last-mentioned mixture had the following water-repellent properties:

AATCC AATCC AATCC Bruehfestig- Spray water permeability (W χ F)

worth lass. '. gkeit tischer < _{Λ l} __

Value ⁱⁿ **

Bleached 70 0 ml 39.9 cm 52.6 χ 32.7 drill

Raw drill 100 41.5 33.8 cm 51.3 x 51 # 3

The steam cured samples had water repellent properties equal to or better than normal were dry cured samples, however, the loss of strength did not occur as with the dry cured samples.

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U69504

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Of course, numerous modifications of the invention are possible Method possible without deviating from the essence of the present invention.

009831/1760

Claims (1)

U69504 (US 301,952 - prio Aug. 14, 1963 - 33 A / B / E / H-7 - 3020) West Point Manufacturing Company
West Point, Georgia, V.St.A. Hamburg, July 27, 1964 Patent claims 1. Procedure for impregnating text !! material! En by Applying an aqueous liquid containing at least one aminoplast and a hardening agent and then soaking it Fixing the aminoplast by warming the textile material before drying, dadursh characterized, that the hardener is a synergistic mixture of at least one acid with one Dissociation constant of more than 10 and at least one ammonia that reacts acidic in an aqueous medium, Amine or metal salt of an organic or inorganic acid is used. 2. The method according to claim 1, characterized in that an at least partially water-soluble condensation product of formaldehyde and melamine or urea is used as aminoplast. -2- 009831/1760 U69504 3H 3. The method according to claim 1 to 2, characterized in that that the aminoplast is fixed on the textile material by steam treatment. 4. The method according to claim 1 to J5, characterized in that dasü aln acid formic acid, sulfamic acid, glycolic acid, Oxalic acid, citric acid, diglycolic acid, tartaric acid, volatile acid and / or orthophosphoric acid are used will. 5. The method according to claim 1 to 4, characterized in that that the salt is a compound of halogen acids, Sulfuric acids, oleohulphuric acids, sulfurous acid, Sulfamic acid; Phosphorous acid, phosphoric acid, fluoroboric acid, Nitric acid, nitric acid, carboxylic acids and / or sulfonic acid is used. 6. The method according to claim 1, characterized in that as hardening agent a mixture of formic acid and magnesium chloride is used. 009831/1760 U69504 7 · Method according to claims 1 to 6, characterized in that the textile material is dried and is treated at an elevated temperature for additional fixation. 8. Method according to Anspiueh 1 to 7 * characterized in that the oils are aminoplasts on textile materials made of cellulose fibers, cotton, synthetic fibers, animal fans or horses in the form of woven, non-woven, knitted or upholstered textiles or from ordered feeers, yarns, Paser heap, staple fibers or individual fibers is applied. 9 «Method according to claim 1, characterized in that that the aqueous impregnation fluid is another one Contains substance that makes the treated textile material waterproof, fire-resistant, resistant to biological Decomposition or biological growth makes or the color, the surface finish, the oriff or the light resistance improves. 009831/1760 H695 (K 10. The method according to claim 1 to 9, characterized in »that the textile material only with the one Aminoplasts and an acid-containing impregnant and then with one containing a salt Means treated. 11. The method according to claim 1 to 9, characterized in that the textile material only with Impregnation agent and a salt and then treated with an acid. 12. The method according to claim 1 to 9, characterized in that the textile material only with Impregnating agent and then impregnated with another agent containing the acid and the salt. 13 · The method of claim 1 to 12, characterized in that one uses an impregnating agent of aminoplasts, acid and sais, still based on the aminoplast used, contains 5 to 50 wt.% Epoxidized triglyceride. 009831/1760 U695CK 14. The method according to claims 1 to 15, characterized in that that the textile material is left in contact with the treatment solution for a long time, so that the aminoplast is exhausted and on the treated textile material deposits. 15. The method according to claim 1 to 14 / characterized in that the treated textile material without intermediate washing is dried. 16. The method according to claim 1 to 15 »characterized in that that the fixation is effected by a steam treatment or by keeping the wet textile material in a moist state. 17 «Method according to claims 1 to 16, characterized in that that the fixation takes place by drying the wet textile material at no more oil at 120 ° C.