DE1218655B - Manufacture of textile fibers or films from mixtures that contain crystalline polyolefins - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

GERMAN

PATENT OFFICE

EDITORIAL

Int. Cl .:

DOIf

German class: 29 b-3/65

Number: 1218 655

File number: M55157IVc / 29b

Filing date: December 17, 1962

Opening day: June 8, 1966

Process for the preparation of basic nitrogen polycondensates in the presence or absence of solvents and condensate agents by reaction of primary aliphatic amines with 3 to 30 carbon atoms or secondary aliphatic amines having 4 to 60 carbon atoms with epichlorohydrin and optionally subsequent further condensation of the product with an or several aliphatic, aromatic or heterocyclic bis-secondary amines are known.

Also the production of textile fibers from mixtures of these polycondensates and with HiKe from stereospecific Crystalline polyolefins, particularly polypropylene, produced by catalysts have already been used described.

In general, the methods for making these textile fibers or films consist of the following Process steps:

1. Mixing the polycondensate (1 to 25% of the total mixture) with the polyolefin on a be ao dear known kind;

2. Granulating the mixture obtained according to 1 at a temperature of 170 to 300 ° C, in screw granulation devices, in order to be able to feed the mixture to the screws of the spinning devices (when using the powdered Mixing is the supply to the screws and therefore the spinning process is not sufficient homogeneous and regular);

3. Compression of the granulate in a melt-spinning device through spinnerets, the holes or have slots whose ratio of length to diameter is preferably greater than 1, and then winding up the spun threads;

4. Drawing and finishing of the threads obtained after 3.

Different polycondensates are used when they undergo drastic thermal treatment Granulation and spinning (stages 2 and 3, above) are subjected to change and show a decrease in their molecular weight as well as a discoloration.

It has now surprisingly been found that the thermal decomposition of dyeable bases is possible Nitrogen polycondensates can be avoided by using the granulation step lets the mixture precipitate and instead proceeds according to the invention.

The subject matter of the invention is a process for the production of textile fibers or foils by melt-spinning mixtures of crystalline polyolefins production of textile fibers or foils from
Mixtures containing crystalline polyolefins

Applicant:

MONTECATINI Societä Generale
per rindustria Mineraria e Chimica,
Milan (Italy)

Representative:

Dr.-Ing. A. v. Kreisler, Dr.-Ing. K. Schönwald,

Dr.-Ing. Th. Meyer

and Dipl.-Chem. Dr. rer. nat. J. F. Fues,

Patent attorneys, Cologne 1, Deichmannhaus

Named as inventor:

Mario Compostella,

Emanuele Del Mauro,

Giovanni Latella, Milan (Italy)

Claimed priority:

Italy of December 21, 1961 (22 809)

and 1 to 25 percent by weight of basic nitrogen polycondensates, those by reaction of primary aliphatic amines having 3 to 30 carbon atoms or of secondary aliphatic amines having 4 to carbon atoms with epichlorohydrin and then Obtained reaction with aliphatic, aromatic or heterocyclic bis-secondary amines have been. The process according to the invention is characterized in that mixtures are spun, which have been sintered at temperatures between 20 and 170 ° C before spinning.

According to the process according to the invention, the mixtures are obtained in the form of grains which have the Screws can be fed to the spinning devices in a regular and homogeneous manner and don't fall apart easily.

To obtain these sintered grains, any apparatus suitable for continuous or batch sintering can be used.

It can sometimes be used to produce dyeable textile fibers based on crystalline polyolefins It may be useful to first prepare a mixture

609 578/514

3 4

bodies that are very rich in basic nitrogen poly- acid black JVS (acidic dye)

is condensate, and then these grains that have a lanasyn red 2GL (metallic dye)

Contains relatively high amounts of polycondensates, to- Setacylgelb 3G (plastic-soluble dye)

together with such an amount of polyolefin grains Cibacet scarlet BR (plasto-soluble dye)

sintering and spinning, which is necessary to produce 5 acetoquinone blue RHO (plasto-soluble dye)

the desired percentage of polycondensates.

in the textile fibers. Example 2

According to the invention, 1 to 50% polycondensate a) From 100 kg of polypropylene, produced with the aid of

first mixed with 99 to 50% polyolefin. of stereospecific catalysts, with a limit

The sintering and spinning according to the invention io viscosity [η] of 1.60 (determined in tetrahydro-

is expediently naphthalene under oxygen-free nitrogen at 135 ° C), a residue after

carried out. Heptane extraction of 94% and an ash content

The threads or foils obtained can finally contain 0.01% and 5 kg of a polycondensate,

colored with acidic or plastic-soluble dyes produced by the reaction of 0.5 mol of n-octadecyl-

will; they also show a good affinity for basic 15 amines with 1.5 moles of epichlorohydrin and 1 mole of piperazine,

and vat dyes. a mixture is made. The mix will

then sintered in a tablet machine; the Ver-

- At s'pi the duration of the mixing of the sintering device is

1 second; in this device the mixture reaches

a) The inventive method 20 a temperature of 100 ° C.

., »_, _,,,"., ".," The sintered tablets are spun in a melt from 100 kg of polypropylene, produced with the aid of a _{spinning device under the} following conditions: from stereospecific catalysts, with an intrinsic viscosity [η] of 1 , 45 (determined in tetrahydro screw temperature .... 260 ° C

naphthalene at 135 ⁰ C), a residue after the head temperature 265 ° C

Heptane extraction of 96% and an ash content spinneret temperature ... 265 ° C

from 0.01% and from 5 kg of a polycondensate, spinneret type 198-0.8-16 mm

produced by reacting 0.3 mol of n-octadecyl maximum pressure 100 kg / cm ²

amine with 1.3 mol epichlorohydrin and 1 mol Piper winding speed 500 m / min,

azin is made a mixture. The mixture _{30 Djb as describedQ} show threads produced

is then sintered in a tablet machine; the _{one Mare color has an} intrinsic viscosity of 85%

Dwell time of the mixture in the sintering direction of _{the original value} .

If the temperature in the device is 1 second _{, the yarns obtained show after} drawing at

tion reaches yo C. _ _ ₁₃ q _{OC in the presence of} steam with a stretching

The sintered tablets are in a melting _{ratio of 1: 5 the following} serimetric

spinning device spun under the following conditions: Properties

Screw temperature .... 250 ° C Tensile strength 6.5 g / den

Head temperature 26O ⁰ C elongation. . . 22%

Spinneret temperature ... 260 ° C ^ cnuuiig ^ _{/ o}

Spinneret type 192 holes with a * ° Immediately after stretching, the

Diameter of threads with a 5% aqueous solution of 0.8 mm and an ethylene glycol diglycidyl ether and then moistened Dried height of 16 mm.

Maximum pressure 100 kg / cm ^{2 b} ) ^On these threads, the following color

Winding speed 500 m / min. 45 fabric stains with good intensity and real

~. . ,,. ,, "_,. to receive:

Show the yarns made as described

a clear color; their intrinsic viscosity is 90% solid yellow 2G (acidic dye)

the original value. Wool red B (acidic dye)

After drawing with alizarin blue, the yarns obtained show ACF (acidic dye)

13O ⁰ C in the presence of steam with an extensible acid black JVS (acidic dye)

ratio of 1: 6 the following serimetric Lanasynrot2GL metallic dye)

Properties: Setacylgelb 3G (plasto-soluble dye)

rj .. ■■,., _c , j Cibacet scarlet BR (plastosoluble dye)

zugtestigjceit ™ g / the acetochinone blue (plasto-soluble dye)

Elongation 20% 55 ^w

Immediately after drawing, the yarn is Example 3

ΐΐϊ ^ ⁵ ° Ä T ^äl i ^rige £ ₊ ^LÖi Tf ^VOn ₊ ^Ät ¥ ^e T *) Made of 100 kg polypropylene, made with the help of

Glykoldiglycidylather moistened and then dried. _of stereospecific catalysts, with a limit

60 viscosity [η] of 1.3 (determined in Tetrahydrob) evidence of technical progress naphthalene at 135 ° C), a residue according to the

AiJ- tj j - * ii j τ- τ- χ cc heptane extraction of 95% and an ash content

These threads are the following dyes _V J _{0Q2g0j and from 5} '£ _a p _o i _ykondensats,

Staining with good intensity and fastness is _produced by the reaction of 0.4 mol of n-dodecyl ^uaite - 65 amine with 1.4 mol of epichlorohydrin and 1 mol of Piper solid yellow 2G (acidic dye) azine, a mixture is produced. The wool red B (acidic dye) mixture is then sintered in a tablet machine; the alizarin blue ACF (acidic dye) residence time of the mixture in the sintering device

Claims (1)

5 6 is 1 second; the mixture reaches 2G in the pre-solid yellow (acidic dye) direction a temperature of 8O ⁰ C. Alizarin blue ACF (acidic dye) The sintered tablets are in a melting acid black JVS (acidic dye) spinning device spun under the following conditions: Lanasynrot 2GL (metallic dye) " _{,, ± ηΛη} οπ 5 Setacylgelb 3 G (plasto-soluble dye) Screw temperature 240 C Cibacet scarlet BR (plastosoluble dye) Head temperature ... 245 C Acetoquinone blue RHO (plasto-soluble dye) Spindle temperature 245 C Spinneret type 198 / 0.816 Maixmaldruck 100 kg / cm ² ₁₀ Claim: Winding speed .... 500 m / min. The threads obtained show after drawing in a process for the production of textile fibers or 130 ⁰ C in the presence of steam with a drawing film by melt spinning of mixtures ratio of 1: 5 the following serimetric of crystalline polyolefins and 1 to 25 Ge properties: 15 weight percent of basic Nitrogen polycondensate Tensile strength 5 5 g / den ^saten ' ^{the durclx} reaction of primary aliphatic Dehnuno- 18 ⁰ I see amines with 3 to 30 carbon atoms ⁰ or of secondary aliphatic amines with Immediately after stretching, the 4 to 60 carbon atoms are epichlorohydrin Filaments having a 25 ° / ₀ aqueous solution of 20 and subsequent reaction with aliphatic, Ethylene glycol diglycidyl ether moistened and then aromatic or heterocyclic bis-secondary dried. Amines have been obtained, thereby g e - b) These threads are marked with the following dye that. one mixes Fabrics dyeings with good intensity and real-time weaves that are made before spinning at temperatures unit: 35 have been sintered between 20 and 17O ^{0 C.} 609 578/514 5.66 © Bundesdruckerei Berlin