DE1260429B - Process for the production of dyed textiles with mouline effect from polyamides - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

GERMAN

PATENT OFFICE

EDITORIAL

Int. CL:

D 06p

German class: 8 m - 1/01

Number: 1260 429

File number: V 26362IV c / 8 m

Filing date: July 14, 1964

Open date: February 8, 1968

The best known processes for the production of textiles with mouline effect are those at which different colored yarns are processed. However, one can also look at the different color affinity make use of different types of yarn and dye the finished textile in one piece. If If you want to use yarns of the same type, that is to say from the same polymer, then you must use suitable yarns Measures one part of it has a higher or lower colorability than the other. It is established been that with polyamides the color affinity for dyes by the addition of so-called Viscosity stabilizers can be varied. Such compounds can be organic acids or Be amines, the polyamide-forming starting materials before the polycondensation in small quantities can be added. Additions of acids, e.g. B. acetic acid, reduce the color affinity, while amines lead to an increase in the color affinity for acidic dyes. It goes without saying, however, that the amounts of stabilizers that can be added to the polyamide-forming starting materials, must not be very large, because otherwise the chain formation is broken off prematurely and end products arise that do not meet the requirements in terms of their thread-forming capacity. if you stay within the limits with the additional amounts that guarantee good spinnability of the polyamides, so that one obtains threads, the textile data of which are acceptable, one can, however, only marginally Achieve color differences.

It has now been found that, in the production of textiles, the tone-on-tone Mou-Iin6 effect in a bath can be dyed, considerable advantages are achieved if one for the production of the textiles, Threads, fibers or yarns made from unmodified polyamides and those made from polyamides that condense from 0.5 to 3 percent by weight of phosphoric or phosphonic acid esters (based on the polyamide-forming Starting material) are modified and / or those made of polyamides, which by condensation from 0.1 to 3 percent by weight isophthalic acid sulfonate or the hexamethylenediamine salt of an isophthalic acid sulfonate (based on the polyamide-forming starting material) are modified, used and the textiles with acidic dyes in a set to a pH of 7.5 to 9.5, preferably 8 to 9 Stains bath.

Polyamides made from caprolactam or from dicarboxylic acids and diamines can be used to produce the polyamide threads. The modified polyamides are produced by the customary polycondensation processes for the production of colored polyamides
Textiles with a mouline effect made from polyamides

Applicant:

Glanzstoff Aktiengesellschaft,

5600 Wuppertal-Elberfeld, Glanzstoff house

Named as inventor:

Dr. Ernst Meyer, 8765 Erlenbach;

Dr. Jürgen Lenz, 8753 öbernburg

The procedure of the above-mentioned starting materials forth, wherein one or 0 _s is added to the condensation approach 0.5 to 3 weight percent of a phosphoric or phosphonic acid ester l to 3 weight percent Isophthalsäuresulfonat or the Hexamethylendiaminsalzes a Isophthalsaäuresulfonats (percent by weight based on the polyamide-forming starting material).

When using caprolactam as a starting material for one with phosphoric or phosphonic acid esters modified polyamide, the addition of a small amount of an aliphatic diamine is recommended, especially hexamethylenediamine. In this case, it is expedient to use 0.3 to 0.5 percent by weight Hexamethylenediamine, based on caprolactam, too.

In addition to the modifying agent, the polyamides modified with isophthalic acid sulfonate can be prepared the caprolactam or AH-SaIz (adipic acid-hexamethylenediamine salt) also has one small amount, e.g. B. 0.1 to 1.0 percent by weight, of an aliphatic diamine, preferably hexamethylenediamine, each based on the polyamide-forming starting material. More expedient however, is the use of the hexamethylenediamine salt of an isophthalic acid sulfonate, one of these Compound an additional amount of 0.5 to 3 percent by weight should be chosen.

The following are particularly suitable for modifying the polyamides: Phosphoric acid esters or phosphonic acid esters the general formulas

XO-P - OX and X-P-OY

I I

OX OY

809 507/596

3 4

in which X is an aryl or alkyl radical and Y is. The carpet shows a 2-colored blue tone in

an aryl, alkyl radical or hydrogen. Clay mouline effect.

For the production of isophthalic acid sulphonate To identify the difference in the intensity of the staining

If modified polyamides are used, it is preferred to be able to determine better strands of thread wise alkali salts of 3-sulfoisophthalic acid, in particular of the polyamides described above, each 3 g

special the sodium salt. in the same bath with the named dye

AUe dyes to be used according to the invention polyamide. The dye picked up by the threads

threads or fibers can be matting agents, as is then done with a pyridine-water mixture

TiO ₂ included. You can also get one of the completely detached. The amount of color is determined by measuring the extinction, customary texturing methods for producing io of the two dye solutions

Crimps, loop formation or the like. Undetermined that are taken up by the thread samples

be thrown. had been. It is noted that the modified

Textiles which, due to the above-mentioned use of polyamide thread 4, absorbed l times as much dye

of threads or fibers made from unmodified and one has like the unmodified,

or two modified polyamides are produced 15.

are woven, knitted and knitted goods of all kinds, example 1

and especially carpets. As described in example 1, there is no modification

A particular advantage of the process is to adorned polyamide made of caprolactam and a modified

see that the textiles are dyed in a bath decorated polyamide made from caprolactam with the addition of

can. Solutions of 1.8 percent by weight ethanephosphonic acid diethyl ester are used as the dye liquor

acidic dyes in water, their pH value and 0.31 percent by weight hexamethylenediamine as well

7.5 to 9.5, preferably 8 to 9, is set. Under a polyamide made of caprolactam with a weight of 1.07

These conditions draw the color to the unmodified percent hexamethylenediamine salt of the sodium iso-

adorned polyamide threads or fibers moderately strong, phthalic acid sulfonate and 0.75 weight percent Na-

made with phosphoric or phosphonic acid esters 25 trium isophthalic acid sulfonate. One multi

modified threads or fibers, on the other hand, have a very high stain, which is produced from the melt of the polyamides

intensively, while the isophthalic acid sulfonate and then subjected to a compression crimping process

holding polyamide threads and fibers became very small, becomes a thread of 3000 denier

Possess capacity for acidic dyes and rotated. A carpet is made from this yarn

practically not stained. You can go through 30, which in compliance with the instructions given in Example 1

Selection of the thread components two- or three-colored given conditions with Telonechtmarineblau G

Manufacture textiles, whereby the dyeings are dyed a good one. The carpet shows a three-colored

Show tone-on-tone shading. Tone-on-tone mouline effect in pale light blue / deep

Especially for carpets that have a jute basic navy blue / cornflower blue. In the case of the above

weave, it is of particular advantage that the investigation of the individual threads

Dyeing in the alkaline range takes place because the amount of ingested dye is found to be

The polyamide modified with isophthalic acid sulfonate does not clean the jute under these conditions

pull on the polyamide threads, as this has been practically not dyed, the other two

is if you look at the dyeing in an acidic ren thread samples as described in Example 1.

pH value. 4 °. . ₁

The method is illustrated in detail by way of examples

explained; A thread made from unmodified polyamide

For example 1 caprolactam and two identical threads made of modified

Polyamide (caprolactam with 2.0 percent by weight

A polyamide is made from caprolactam after the 45 phosphoric acid triethyl ester and 0.31 percent by weight

customary polycondensation process and hexamethylenediamine) are twisted together,

spins this into multifilament threads with a titer of. This is used to make a carpet, which then

1000 den (72 single threads). In an analogous manner, poly- colored using anthralan blue B,

if caprolactam is condensed with the addition of The conditions for dyeing correspond to those,

1.8 percent by weight of ethanephosphonic acid diethyl ester 5 ° which are given in Example 1, with the exception

and 0.31 percent by weight hexamethylenediamine (by setting the bath to a pH of 9

gen related to caprolactam) and represents from the becomes. The colored carpet shows a two-tone one

modified polyamide produced in this way, likewise blue tone-on-tone mouline effect. By extink

a multifilament thread with a titer of 1000 den (72 individual measurement is determined that the modified

threads). Two threads made of unmodified polyamide have absorbed 3.2 times more dye

amide and a thread of modified polyamide as the unmodified,

are textured by upsetting pucker and then. .

Twisted together with a thread of 75 S. From the example

the resulting 3000 denier yarn is tufted. A modified polyamide is made from Caprolac-

Carpet using a jute fabric. The 60 camouflage with 0.75 percent by weight phosphoric acid triethyl

finished carpet is in an aqueous bath, the ester and spun this into a thread cable,

1% Telonechtmarineblau G contains, at a pH that is then crinkled and stacked to length

Value of 8.5 and a temperature of 100 ° C is cut. The resulting fibers are with

Dyed on a reel skid for 1 hour. The fibers made of unmodified polyamide from Capro-

Liquor ratio is 1:50. After completion 65 lactam processed together to a yarn, and

In terms of color, the modified polyamide yarn has a mixture of 2: 1. The fiber yarn

deep navy blue coloring ingested during the one used to manufacture a fabric in

Unmodified portion of corflower blue has become body weave. One stains using a

aqueous dye liquor containing 1% anthralan blue B, at a pH of 9. The fabric shows a blue two-color Mouline effect. Through the The extinction measurement explained above shows that the modified polyamide has 1.7 times as much dye recorded like the unmodified.

Example 5

Made from a fiber yarn made of 1 part unmodified polyamide made from adipic acid and hexamethylenediamine and 2 parts of modified polyamide from the same starting materials with 0.74 percent by weight Phosphoric acid triethyl ester is used to produce a fabric. This is described in the above Wise colored with Telonechtmarineblau G at a pH value of 8.5. It then shows a blue one Tone-on-tone mouline effect. The modified polyamide absorbs 2.2 times as much dye as it does not modified.

Example 6

A fiber yarn is produced from unmodified polyamide fibers from adipic acid-hexamethylenediamine and those obtained by condensing in 2.22 percent by weight of sodium isophthalic acid sulfonate and 0.96 percent by weight of hexamethylenediamine and those that are modified by condensation are modified by 2.4 weight percent phenylmethanephosphonic acid diethyl ester. The yarn processed to a fabric which is then dyed with anthralan blue B at a pH of 8 will. A three-tone mouline effect is obtained. While that modified with the isophthalic acid sulfonate Polyamide absorbs practically no dye, the color uptake is the one with the phosphonic acid ester modified material 3.5 times as much as that of the unmodified polyamide.

In addition to the dyes already mentioned in the examples, when using the dyes according to the invention Mixtures of threads etc. from modified and unmodified polyamides Mouline effects Achieve with all acidic dyes if you use the textiles produced in a manner known per se stains in a bath while observing the pH value limits of 7.5 to 9.5. The optimal conditions during the dyeing process with regard to the liquor ratio, the temperature, the duration of the dyeing and the pH value can easily be carried out through a preliminary test for the respective mixture of the textile material and the dye determine. The following acidic dyes can also be mentioned in detail: Acilan marine blue, Acilan Navy Blue B, Alizarin Cyanine Green, Alizarin Cyanine Green 5 G, Acilan Naphthol Red G, Acilan Ponceau GBL, Diacilangrenadin S, Acilanorgane GX.

Claims (3)

Patent claims: 1. Method of making in tone-on-tone moulino dyed textiles made of polyamides by single-bath dyeing, characterized in that that one for the production of textiles, threads fibers or yarns from modified Polyamides and those made of polyamides, which by condensing in from 0.5 to 3 percent by weight Phosphoric or phosphonic acid esters (based on the polyamide-forming starting material) modified are and / or those made of polyamides, which by condensing in from 0.1 to 3 percent by weight Isophthalic acid sulfonate or the hexamethylene diamine salt of an isophthalic acid sulfonate (based on the polyamide-forming starting material) are modified, used and the Textiles with acidic dyes in a bath set to a pH of 7.5 to 9.5 stained. 2. The method according to claim 1, characterized in that for the production of the textiles, Threads, fibers or yarns made from unmodified polyamides and those made from polycaprolactam, the by condensing in 0.5 to 3 percent by weight of a phosphoric or phosphonic acid ester with the addition of 0.3 to 0.5 percent by weight of an aliphatic diamine (quantities in each case based on caprolactam) modified is used. 3. The method according to claim 1, characterized in that for the production of the textiles, Filaments, fibers or yarns made from unmodified polyamides from 0.1 to 3 percent by weight of one Isophthalic acid sulfonates with the addition of 0.1 to 1.0 percent by weight of an aliphatic diamine (Amounts in each case based on the polyamide-forming starting material) modified are used. 809 507/596 1.68 © Bundesdruckerei Berlin