DE1469111B - Process for the production of high-strength threads from crystalline polyolefins - Google Patents

Description

The invention relates to a process for the production of mono- and plurifiles from crystalline ones Olefin polymers and in particular from polypropylene made with stereospecific catalysts according to the melt spinning process.

In previous proposals, the production of mono- and plurifiles by extrusion of olefin polymers, in particular polypropylene, already described in the molten state. The ones after the known The mono- and plurifiles obtained by the process already have a considerable tensile strength, but they do generally does not exceed 6 to 7 g / den.

The object of the present invention was now to provide polyolefin threads with an even higher tensile strength to create.

The invention relates to a process for the production of high-strength threads based on crystalline polyolefins, optionally color modifiers, stabilizers, matting agents, pigments or contain dyes, by melt spinning and subsequent drawing, thereby is characterized in that the emerging from the nozzle threads through an immediately behind the Spinneret arranged tubular device heated to temperatures in the range between 130 and 300 ° C, whose diameter is 2 to 5 cm larger than that of the spinneret and which is 2 cm to 1 m long, then leads with stretching ratios between 1: 2 and 1:10 at temperatures between 80 and 150 ° C in hot air, Steam or similar medium heated stretchers or heated platen stretched and, in the case of the use of polyolefins containing color modifiers, the threads optionally before or after stretching with formaldehyde, isocyanates or diepoxy compounds treated.

The process according to the invention can be used both on polyolefins alone and on mixtures of polyolefins with additives such as color modifiers, stabilizers, matting agents, pigments or dyes, be applied.

It is preferred to use essentially isotactic polypropylene as the crystalline polyolefin an intrinsic viscosity between 2 and 5.

Color modifiers are preferably obtained by condensation of epichlorohydrin with amines basic nitrogen compounds are used, while a stabilizer from 0.02 to 2 percent by weight, based on the polymer, an aliphatic thioester, a dialkylphenol sulfide

table

Composition of the mixture example 1 Example 2 a) polypropylene 7o
Intrinsic viscosity (determined in tetrahydronaphtha
linbeil30 ° C)
Ash content
Residue after heptane extraction
b) Calcium stearate ° / o
c) Stabilizer 7 "
Lauryl thiodipropionate
4,4'-thio-bis-3-tert. butyl metacresol
Spinning Conditions:
Screw temperature
Spinning head temperature
Spinneret temperature
Spinneret type
Temperature of the heated tubular device
below the spinneret
Maximum pressure (kg / cm ² )
Winding speed (m / min.)
Stretching conditions:
temperature
medium 3.00
0.01%
94.00%
0.3
0.6
0.2
230 ° C
235 ° C
285 ° C
40 / 0.8 -16 mm
160 ° C
30th
600
130 ° C
steam
1: 8.3
9
18th 2.50
0.027,
94.5%
0.3
0.6
0.2
230 ° C
230 ° C
270 ° C
40 / 0.8 x 16mm
140 ° C
25th
600
130 ° C
steam
1: 8.5
8.8
20th Stretch ratio
Properties of the drawn fiber:
Tensile strength (g / den)
Strain (%)

1 469 ΠΙ

3 4

and calcium stearate consisting mixture preferably a melting point of 17O ⁰ C, a specific

will. Weight of 0.915 and a crystallinity

After stretching, the threads can be thermally through X-ray examination, from 50% in

see shape stabilization treatments under conditions - a Henschel mixer with 30 g calcium stearate,

free or hindered shrinkage 5 60 g lauryl thiodipropionate and 20 g 4,4'-thio-bis-

as well as the usual final treatments. 3-tert. butyl metacresol mixed. Then will

Modifiers of the mixtures of polyolefins with dyeing the mixture in a Werner extruder at 210 ° C filaments obtained can be further granulated and the granules in a Schmelzspinnvor or after stretching, for example, molding apparatus at a screw temperature of 230 ⁰ C, aldehyde Allow diisocyanates or diepoxy compounds to act at a spinning head temperature of 235 ° C and a spinning head. nozzle temperature of 285 ° C melt-spun. the

The invention is used in the following Example 1 spinneret had 40 bores, each

as well as the other tabular compiled a diameter of 0.8 mm and a length of

Examples explained. Example 6 shows the critical 16 mm. The temperature of the heated

Limit of the treatment according to the invention. Above the tube below the spinneret was 160 ° C.

Surprisingly, it was found that a manual press was carried out with a maximum pressure of 30 kg / cm ² ;

Development below 130 ° C in a noticeable way the pulling speed was 600 m / min. The

reduces the strength of the polypropylene fibers. Spun yarn was then spun at 130 ° C in the presence of steam with a draw ratio of 1: 8.3

B is ρ ie 1 1 ² ° stretched. The drawn yarn had the following mechanical properties:

890 g of crystalline polypropylene of a limiting viscosity

did, determined in tetrahydronaphthalene at 135 ° C, ^age 5.04 den

of 3.00, an ash content of 0.01%, a back tensile strength of 9 g / den

after extraction with n-heptane of 94 ° / ₀ , ^a 5 elongation 18%

Example 3 Example 4 Example 5 Example 6
(Comparison) 3.00 3.00 2.00 3.00 0.01% 0.04% 0.02% 0.01% 94.00% 95.6% 96.1% 94.00% 0.3 0.3 0.3 0.3 0.5 0.6 0.5 0.6 0.2 0.2 0.2 0.2 23O ⁰ C 240 ° C 230 ° C 230 ° C 230 ° C 24O ⁰ C 240 ° C 235 ⁰ C 250 ° C 295 ° C 285 ⁰ C 285 ° C 50 / 1.3 x 26 mm 20 / 0.4-8 mm 20 / 0.4-0.8 mm 40 / 0.8 x 16mm 130 ° C 280 ° C 270 ° C 11O ⁰ C 30th 45 35 30th 80 240 320 600 150 ° C 130 ° C 135 ° C 13O ⁰ C steam Warm air Warm air steam 1:10 1: 6.28 1:10 1: 8.3 9.5 14.5 11.5 5.8 12th 23 20th 14th

Claims (3)

Patent claims: 1. A process for the production of high-strength threads based on crystalline polyolefins, which optionally contain color modifiers, stabilizers, matting agents, pigments or dyes, by melt spinning and subsequent drawing, characterized in that the threads emerging from the nozzle through a directly behind the Tubular device arranged in a spinneret and heated to temperatures in the range between 130 to 300 ⁰ C, the diameter of which is 2 to 5 cm larger than that of the spinneret and 2 cm to 1 m long, conducts, then with stretching ratios between 1: 2 and 1: 10 stretched at temperatures between 80 and 150 ⁰ C in stretching devices heated with hot air, steam or a similar medium or over a heated plate and, in the case of the use of polyolefins containing color modifiers, the threads optionally treated with formaldehyde, isocyanates or diepoxy compounds before or after stretching . 2. The method according to claim 1, characterized in that the crystalline polyolefin is im essential isotactic polypropylene with an intrinsic viscosity between 2 and 5, determined in Tetrahydronaphthalene at 135 ° C was used. 3. The method according to claim 1 and 2, characterized in that one uses polymers which ^{contain mixtures of 0.02% emes} aliphatic thioester, a dialkylphenol sulfide and calcium stearate as a stabilizer.