DE1669418C3 - - Google Patents

Description

OR ₂

wherein R is hydrogen, methyl or the group

R, hydrogen or the —SO ₃ Na group and R ₂ hydrogen, the group

or

Eevenness and depth of color leave much to be desired, as some dyes have an increasing efinket with increasing concentration. In terms of inorganic color pigments, practically only ultramarine, Cadmium sulfide, iron oxide and chromium oxide for spinning dyes are usually taken into consideration Polyamide chips are colored by treating them with dye solutions or dye dispersions and after drying after the melt spinning process drive spun into threads. In this trial there is no continuity and at the same time: a increased expenditure on equipment required.

In French patent specification 1,149,967 svird mentions that brominated anthraquinone disulfone

acids are suitable for dyeing artificial nitrogenous fibers. However, from this information cannot be concluded that the polyamide dye concentrates according to the invention, their dyes not with in the French patent 1 149 967 be writings are identical, too surprisingly better ten results, especially with regard to the stability of the dyes, under the extreme conditions melt extrusion. There has now been a process for spin dyeing Shaped structures produced by the melt spinning process from linear, synthetic polyamides by anthraquinone dyes which are soluble in polyamide, which is characterized in that one anthraquinone dyes of the formula

O NH-R

³⁵ OR ₂

wherein R is hydrogen, methyl or the group 40

denotes where A is a divalent linear or branched alkyl radical, homogeneously distributed in part of the polyamide to form a dye _{concentrate, R 1 is} hydrogen or the —SO ₃ Na group and R _{2 is} this dye concentrate mixed with the majority of the hydrogen, the polyamide group and then this mass ^ ~~ V

melt spinning. - NH-CJ / - ^CH 3

2. The method according to claim 1, characterized in that 0.1 to 20 percent by weight of or

Concentrate, based on the total amount of 50 NH ₂

spinning mass, adds.

55

The invention relates to a process for spin-dyeing by the melt-spinning process manufactured molded structures from linear, synthetic polyamides.

It is known to dye synthetic polyamides in bulk, with inorganic or organic Dyes or pigments are used. Due to the high melting temperature of the polyamides, the choice of dyes is very limited. A number of metal complexes of azo dyes and phthalocyanine metal complexes have been proposed. However, durability, light

-NH

means where A is a linear or branched alkyl radical, homogeneously distributed in part of the polyamide to form a dye concentrate, this dye concentrate is mixed with the majority of the polyamide and then this mass is melt-spun. It was found that these dyes are surprisingly stable and lightfast at the given process temperatures. The following anthraquinone dyes are suitable:

3 Formd H ₂ N O
Il 4th hue X JU O
π NH ₂ SO ₃ Na NaO ₃ S ^ ν Jv I.
HN
/ Il
O blue γρ
Vy ι Τ J Il
O ι
NH
V I. \ /
CH ₂ O- ^ch > O
Il NH-
I. green Ca ' / \
Y Y> CH _S Ii
ο T
NH-

The color concentrates are prepared in such a way that they preferably contain 5 to 30 percent by weight of dye contain. To produce them, the dye powder can be mixed with a polyamide granulate and homogenize the mixture in a heated extruder, whereby the color concentrate melt advantageously processed into granules. amides the processing temperature in the extruder can be reduced considerably.

In a special embodiment of the process, the dye or the dye mixture is used or a dye solution in which the dye in 4 = a solvent compatible with polyamide, e.g. B. EthylglykoL is dissolved, stirred into a previously prepared polyamide or mixed polyamide melt with exclusion of air, the solvent being evaporated again when a dye solution is used and the color concentrate melt, which is homogeneous after the dye has dissolved, is processed into granules When producing polyamide or mixed polyamide melts, matting and / or color pigments can also be used.

The dye concentrate granulate can either be spun as a mixture with normal polyamide granulate or added to a continuously produced polyamide melt via a melting and metering device before spinning. Generally, dye contents of about 0.01 to 2.0% are required in the shaped articles. The dye concentrates can also be used as a mixture with matting or colored pigment concentrates will.

Coloring and / or matting pigments can also be added to the starting materials before the polymerization Anti-aging agents, viscosity stabilizers, etc. are added.

By spectrophotometric extinction measurement of the dye concentrate solution in cresol in comparison with the dye solution can be detected be that under the mild processing conditions at 200 ° C even after an easterly residence time in no detectable dye degradation has occurred in the mixed polyamide melt

example

Preparation of a dye concentrate in an extruder 15 parts by weight of an anthraquinone dye of the formula

O NH ₂ H ₂ NO

are mixed with 85 parts by weight of polyamide 6 granules (relative viscosity 1 g / 100 ml in cresol = 2.70)

and processed in an extruder at 250 ° C to a homogeneous melt and then to granules. If you use a polyamide with the solution viscosity, 2.0, the processing temperature can be reduced to about 220 ° C.

Example 2

Production of a dye concentrate

in the autoclave

In a stirred autoclave made of stainless steel, a composite polyamide 6/66 85 percent by weight / 1 5 weight percent adipate hexanediammonium by polycondensation appropriate amounts caprolactam and produced under pressure at 250 ⁰ C in a known manner. After releasing the pressure, the temperature of the mixed polyamide melt is reduced to about 200 ^° C. and an anthraquinone dye according to Example 1 is added with the exclusion of air, so that the color concentrate melt contains 15 percent by weight of dye. After about an hour, the dye has distributed homogeneously in the melt. The processing to granulate can be done according to a dry or wet spinning process.

By increasing the amount of dye added, a dye containing 20 percent by weight can also be added Make concentrate.

Example 3
Manufacture of dyed threads

In a spinning apparatus heated to 260 to 270 ° C, which is equipped with a mixing roller, a mixture of 6.7 parts by weight of the dye concentrate is 15% (prepared according to Example 1 or 2) and 933 parts by weight Polyamide 6 granules too deep blue colored Threads with a final titer of 90/25 den spun. The light, washing, sweat, chlorine, rubbing, dry cleaning, The threads are very fast to iron and acid

If a mixture of 0.67 parts by weight of color concentrate and 99.4 parts by weight of polyamide granulate is used, in this way, light blue colored threads with correspondingly good coloristic fastness properties are obtained.

Claims (1)

Patent claims: 1. Procedure for spinning dyes from after Molded structures made of linear, synthetic polyamides produced by melt-spinning processes with the aid of anthraquinone dyes soluble in polyamide, characterized in that that one anthraquinone dyes of the formula NH-R