DE1669455A1 - Mixed polyamide threads resistant to color - Google Patents

Description

PATENTANWÄLTE M O N C H E N 5 DR.-ING. H. FIMCKE MÜLLERSTR. 31 D ι ρ L.-1 ν G. H. β ο η R 16. Sep. 1966 DIPL.-ING. S. STAEGER

Folder 20942

Case Noα FO 18725

description

to the patent application

of Finta HiFERIAL CHlSfICAL INDUSTRIES LIMITED, London S.W.1, GREAT BRITAIN,

concerning

"Color-resistant mixed polyamide threads ¹¹ "

PRIORITY: September 16, 1965 - UK.

The present invention relates to threads made of micropolyamides, which resist coloring by external or basic dyes

Polyamide yarns and goods made from them are usually used colored with emulsion dyes or acidic dyes, while basic dyes are rarely used that not all yarns used are dyed to the same extent by one of the above classes of dye, so that, for. B.

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Contrast dyeing and other effects can be achieved when dyeing the pieces ₉ To achieve these effects, some polyamide yarns are modified, e.g. B. a chemical manner to staining by usual _s acidic dyes to widerstehenο Such yarns as "resistant to staining" yarns are known. It is of course important that the modifications made to the yarns in no way detract from their desired characteristics and that the physical properties of the various yarns be as identical as possible.

Ih the patent specification (patent application of the same

Applicant dated September 15, 1956 with the title "Polyamide fibers", internal file number cap 20939 Case No. FC 18724) describes that certain mixed polyamides can be produced ₉ which, although they have practically the same softening points as polyhexamethylene adipamide, have considerably higher melt viscosities at the same or almost the same molecular weight.

The copolyamides mentioned are ternary copolymers of polyhexamethylene adipamide and polyhexaethylene terephthalate together with a smaller proportion of a third component, such as polyhexamethylene isophthalamide or poly- ε-caprolaotam.

It has now been found that the molecular weight of this ter-

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Nary mixed polyamides by adding relatively large amounts of a molecular weight stabilizer, e.g. B. one Acid, can be lowered without affecting the melt viscosities of it to be reduced to an extent at which it does not work Can be spun into clay, as is usually the case Case would be. Those made from mixed polyamides in the presence of a relatively large amount of an acidic stabilizer are made by the normal Terfehren of the Schmelespinnene The threads obtained by drawing and drawing are resistant to acid dyeing. The use of correspondingly large quantities an alkaline stabilizer would of course make the yarn resistant to alkaline dyeing o such threads would be Of course, also valuable for deeply colored threads, as the large number of these as a result of the addition of a basic stabilizer the available amino end groups would make the threads particularly suitable for acid dyeing «

Accordingly, the present invention provides a process for producing polyamide filaments by melt spinning and subsequent cold drawing of a mixing polyamides having a Sohmelsviskosltät of at least 40 P at 39O ⁰ C, said composite polyamide at least 50 wt _o - $ Folyhexamethylenadipamid together with 20-40 wt «# polyhexamethylene terephthalate. and 2-20% by weight of a third polyamide and by polymerizing a mixture of Hexamethylendiammoniuaadlpat »Hexamethylendiammoniumterephtahalat and a third

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th polyamide-forming salt or lactam in the presence of a Equivalents of at least 3 * 0 moles # of a monofunctional acidic or basic stabilizer, is «

Of course, the expression "equivalent of at least 3.0 mol% of a monofunctional acidic or basic stabilizer ¹¹ includes a difunctional stabilizer which is present in a slope which is equivalent to at least 3 * 0 mol% of a monofunctional stabilizer»

The term "stabilizer" is to be understood as an acidic or basic compound, for example acetic acid, which normally is added to a polyamide-forming salt to control the molecular weight thereof.

The third polyamide-forming salt or lactam in the mixture preferably makes up 5-10 % of the same and is hexamethylene diammonium isophthalate or i-caprolactamo. The stabilizer can be an acid and is preferably a dibasic acid such as adipic acid or terephthalic acid

The following examples explain the process according to the invention without restricting it.

BEISFIFX 1

A ßnlzgemiecb _s the hexamethylenediammonium, hexamethylene "lendiammoniumterephthalat and caprolactam in a molar ratio

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from 60/30/10 together with; Containing 2 mol% of terephthalic acid stabilizer, the polymerization was carried out as follows: 1726.5 g of the above mixture were introduced into an autoclave together with 1000 g of water and kept under a nitrogen atmosphere. The temperature of the mixture was increased to 150 ° G within an hour and 40 minutes, during which time the pressure rose to 1.6 atmospheres. The pressure was kept at this value for one hour, during which the temperature rose to 24-5 ⁹ C , and then reduced to 0 atm over the course of one hour with a temperature increase to 285 ° C. Finally, the mixture was kept at 293 ° C for one hour Steam kept at atmospheric pressure and the mixed polyamide then extruded into cold water. The "Sew"% ratio of the polyamide components, based on the finished mixed polyamide, was 61.7 / 33.1 / 5 * 2.

The properties of the resulting mixed polyamide are given in Table I below *

TABLE I.

Properties of 6 * 6/6 T / 6 mixed polyamide. that with 2 mol% Terephthalic acid stabilizes 1st

Amino end group equivalents per 10 ⁶ g 18.7 carboxyl end group ^{equivalents per 10 6} g 183 5 Melt viscosity 385 P at 300 ° C

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Bas polymer was chipped and at 290 ⁰ C to a sechsfädigen yarn having filaments of circular cross-section spun "The filaments were wound up at ca" 24-0 m / min, and then at a draw ratio of 4.6 on a hot plate at 100 ° C Drawn The properties of the drawn yarn are given in Table II below

TABLE II
Properties of drawn 66/6 T / 6 mixed polyamide yarn

Denler count after stretching 98.1. Strength (g / den) 4.57

Elongation at break (%) 21.5 Initial modulus (g / den / 100 % ^T. Idea) 22.0 Shrinkage in boiling water (%) 16 Amino end group equivalents per 10 g of 12.5 Carboxyl end group equivalents per 10 g of 166.1

The yarn was made on a Ilingstrumpfmaschiae together with a nylon 66 control and the fabric became a Solway Blue B colored. There was a pronounced color difference between the samples, and after over-dyeing with Dispersal Fast Yellow A. (Dispersal Fast Yellow A) was the pattern, which contained the Miechpolyergarn, yellow, and the nylon 66 control oyster green.

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EXAMPLES 2 and 3

Sals mixtures, the hexamethylene diamaonium adlpat, hexamethylene diammonium terephthalate and oaprolactam in a molar ratio Tone 60/30/10 together with water and 1.8 or 2.5 mol pounds Adipic acid stabilizer were used according to the example .1 method described polymerized.

The properties of the mixed polyamides formed are given in Table III below.

TABLE III

Properties of 6 * 6/6 T / 6 mixed polyamides that stabilize _{old I 0} 8 or 2.5 mol * adipic acid

Amino end group equivalents per 10 g 19 15 Carboxyl end group equivalents per 10 g of 1? 3 "0 229 SehmelzviskositSt 1200 F 1300 F

at 290 ⁰ C at 29O ⁰ C

Threads spun from the copolymers were resistant to acidic dyeing «

EXAMPLE 4

The Miechsalz of Examples 2 and 3 was together with 2.25 Hexamethylenediamine as a basic stabilizer and water-absorbing agent

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polymerized ter the conditions described in Example 1.

The properties of the mixed polyamides formed are in the given in Table IV below «

Properties of 6 »6/6 T / 6 mixed polyamide. the bit 2 mole # Hexamethylenediamine is stabilized

Amino end group equivalents per 10 g 1J2 Carboxyl end group equivalents per 10 g 16 Melt viscosity YW? F at 290 ⁰ C

Threads spun from the mixed polymer were resistant to basic dyes, but dyed well with acidic ones Dyes

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Claims (1)

PATENT CLAIMS 1c) Process * ur production of drawn polyamide threads by narrow a ep inside a mixed polyamide with a viscosity of at least 400 P at 290 ⁰ C and subsequent cold stretching of the spun threads "characterized in that the mixed polyamide together with at least 30% by weight of polyhexamethylene adipamide 20-40 wt .-% polyhexamethylene diammonium terephthalate and 2-20% by weight of a third polyamide and comprises by polymerizing a mixture of hexamethylene diammonium adipate * hexaaethylene diammonium terephthalate and a third polyamide-forming salsa or lactams in the presence of an equivalent of at least 3.0 Uol% of one monofunctional acidic or basic stabilizer is formed. 2 · The method according to claim 1 »characterized in that the mixture contains 5-10% by weight of the third polyamide 3 · The method according to claim 1 or 2 «characterized in that that the third polyamide sais or lactam is hexamethylene diammonium isophthalate or f-caprolactam is used « 4, method according to one of the preceding claims · «thereby characterized in that an acid is used as a stabilizer ο 909842/1667 5o method according to claim 4-, characterized in "that as acid adipic acid or terephthalic acid used v / irdo 6 «Method according to one of claims 1 ~ 3 _3, characterized in that hexamethylenediamine is used as the stabilizer. PATBiTANWXLTi DIHHQ. H. FiNCKE. DIPl ING H. BOHB
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