DE1217544B - Process for the production of fibers from hydrate cellulose - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

GERMAN

PATENT OFFICE

EDITORIAL

Int. CL:

DOIf

German KL: 29 b -3/20

Number: 1217 544

File number: C21918IVc / 29b

Filing date: July 15, 1960

Opening day: May 26, 1966

It is known that fibers or films made from hydrate cellulose to be prepared by pouring viscose through nozzles or slots into, preferably acidic, saline Baths presses. The procedure has been modified many times. This modification served mainly the purpose of facilitating the process management and / or the quality of the process-based To improve fibers or foils.

A frequently practiced modification is that one uses substances that make the production facilitate the viscose, e.g. B. in xanthogenation by emulsification of carbon disulfide the xanthogenate formation Shorten and / or finely disperse accompanying substances in the viscose so that ζ. Β. a flawless one Filtration is guaranteed. Additives can also improve their thread-pulling ability to make noticable. Furthermore, the annoying deposition of impurities from the Viscose and / or from the spinning bath at the spinnerets can be avoided. The spinning baths remain as a result of the products added to them or those which enter them from the viscose, they are free of otherwise customary sedimenting opacities. As substances that are used to achieve the aforementioned effects of viscose and / or can be added to the spinning bath are up to now in addition to sulfonated and sulfated oils among other things, oxyethylated amines and pyridine compounds became known.

As is known, rayon threads with particularly good performance properties are obtained when viscose is used spun, obtained from cellulose with a higher average degree of polymerisation are. However, such viscoses have a higher viscosity. To be able to spin such viscose, you have to bring it to a higher temperature so that the viscosity is lower.

With the previously known surface-active viscose additives, which contain basic nitrogen, but the problem occurs at temperatures above 40 ° C one that they no longer remain clearly soluble in the viscose or in the spinning bath. With this undesirable If the solution state changes, they lose their effectiveness during the spinning process.

The subject of the invention is a method for producing fibers from hydrate cellulose by spinning viscose in a spinning bath. The process according to the invention is characterized in that a viscose is spun, either this and / or the spinning bath being amine oxides of the general formula R ₁

Method of making fibers from
Hydrate cellulose

Applicant:

Chemical factory Stockhausen & Cie.,
Krefeld, Bäkerpfad 25

Named as inventor:

Dr. Eduard Barthell,

Dr. Hermann-Dietrich, Schmidt-Neuhaus;

Friedrich Hilgers, Krefeld

R ₃

in which R ₁ , R ₂ and R _{3 are} alkyl or aryl radicals.

Suitable amine oxides are, for example: dimethyl lauryl, Diethyloctyl, tributyl, dimethylbutyl, triisopropyl, triisooctyl, methoxyethylmethyllauryl, Dimethylstearyl, diethyl oleyl, dimethylcyclohexyl, dicyclohexylmethyl or dimethylphenylamine oxydi

Of particular advantage is the fact that all of the compounds mentioned are added to the viscose causes the improvements outlined above. The viscose is clarified and its filtration capacity is improved. By reducing the interfacial tension, a better thread-pulling ability is achieved and better spinnability. When spinning viscose, which have a high viscosity, can these, without the compounds mentioned according to the invention precipitating, are heated to such an extent that they can be easily spun and produce fibers with particularly high strength.

example 1

A viscose of the composition:
8.1% cellulose,
6.3% NaOH,

32.0% carbon disulfide, based on cellulose,

Viscosity: 93 seconds ball drop,
0.2 g of dimethyllaurylamine oxide are added per liter. The effect of the addition is that the viscose becomes clear, translucent, can be filtered easily, has excellent thread-pulling properties and its surface tension is reduced by at least 50%

609 570/515

will. At a spinning maturity of 12 ° Ho this viscose is spun on a centrifuge spinning machine. The spinning bath has the following composition:

10

12OgH ₂ SO ₄ Ί
24OgNa ₂ SO ₄ > per liter.
8 g ZnSO ₄ J

The temperature is 50 ⁰ C.

The spinning is done with 24-hole nozzles; the spun silk has a denier of 120 denier.

In order to be able to spin a viscose with such a high viscosity, it is necessary to heat it ^{to about 40 ° C. before spinning.} During this heating process, the viscose retains the properties described above without becoming cloudy.

No nozzle incrustation occurs when the viscose is spun, and the precipitation bath is not contaminated due to sulfur-containing compounds does not occur.

Example 2

If, as in Example 1, a viscose is processed instead of a maturity of 12 ° Ho with a maturity of 18 ⁰ Ho using 0.8 g diethyloctylamine oxide per liter of viscose, the effects mentioned in Example 1 are also achieved, and In addition, the milkiness that always occurs when processing unripe viscose is avoided.

Example 3

One intended for the production of cord threads Viscose of the following composition:

in addition, a surprisingly high stretchability of the rayon is achieved. That after this spinning process produced cord paleon has a conditioned strength of 4.8 g / den and an elongation 5 out of 12%.

Example 4

A viscose of the following composition commonly used in the manufacture of cord threads:

6.75% cellulose,
5.80% NaOH,
45.00% carbon disulfide based on

Cellulose,
1.00% methylcyclohexylamine,

Viscosity: 80 seconds ball drop, is spun at a gamma value of 47 on an industrial rayon machine according to the super cord spinning scheme.
The spinning bath has the following composition:

in liter.

30th

6.67% cellulose,
5.79% NaHO,

38.00% carbon disulfide, calculated on cellulose,

35

on

Viscosity: 280 seconds dropping a ball, adding 2 g of tributylamine oxide per liter. These Viscosity is measured at a gamma value of 47 on an industrial rayon machine according to the super cord scheme spun. The spinning bath has the following composition:

45

6OgH ₂ SO ₄ 1
8OgZnSO ₄ \ per liter.
12OgNa ₂ SO _{4 y}

Temperature: 42 ° C.

A gold-platinum nozzle with 1000 holes, 60 μ is used as the spinneret. Diameter. The cordreyon is drawn in a second spinning bath, which contains 25 g of H ₂ SO ₄ per liter, at a temperature of 96 ° C. by 120%.

In order to be able to spin such a viscose at all, it is necessary to heat it to a temperature of about 60.degree. The viscosity drops to about 80 seconds as a ball falls. The amine oxide incorporated in the viscose remains clearly dissolved in the viscose and fully effective, so that the intricate spinning process runs smoothly and 60 g of H ₂ SO ₄
70 g ZnSO ₄
120 g Na ₂ SO ₄
0.5 g diethyllaurylamine oxide

Temperature: 43 ° C.

A platinum-iridium nozzle is used as the spinneret with 1100 holes and 50 μ nozzle hole diameter.

The spun in this spinning bath Kordrayon is stretched in a second spinning bath containing 25 g of H ₂ SO ₄ per liter at a temperature of 98 ⁰ C to 110%.

It is known that spinning with spinning baths which have a high zinc sulfate content is very easy Incrustations arise on the nozzle holes and on the thread guide elements. In addition, there is the decrease in viscose at the spinneret, caused by the high gamma value of the viscose and the low Sulfuric acid content in the spinning bath, very bad. By adding diethyllaurylamine oxide to the spinning bath the interfacial tension of the spinning bath is reduced more than with the means previously used was known, which in turn improves the removal of the viscose from the nozzle and also improves the Formation of incrustations can be prevented.

Claims (1)

Claim: Process for making fibers from hydrate cellulose by spinning viscose in one Spinning bath, characterized in that a viscose is spun, either these and / or the spinning bath amine oxides of the general formula Riv in which R ₁ , R ₂ and R _{3 are} alkyl or aryl radicals. 609 570/515 5.66 © Bundesdruckerei Berlin