DE1084231B - Process for the antistatic finishing of polyethylene terephthalate threads or fibers - Google Patents

Description

The invention relates to a method for aftertreatment of polyethylene terephthalate threads or fibers with a softener, which the threads or fibers and the textiles made from them have good antistatic properties in addition to a pleasant feel confers. By reducing the electrostatic charge on the fibers, their mechanical workability, z. B. when carding, carding, drawing or spinning, significantly improved.

It is known that cation-active compounds with surface-active properties are used for the aftertreatment of artificial fibers. It has also been proposed to use anion-active compounds with a more or less acidic character as a preparation or softening agent for synthetic threads or fibers. These compounds, which form anion-active colloidal electrolytes into high molecular weight hydrophobic molecules through the entry of negatively charging groups such as —O ₃ H, —O — SO ₃ H, —O — PO ₃ H _{2, have different properties of textiles depending on their structure} Aids.

Neutral addition products of alkylene oxides with an acidic one are also used as antistatic agents Alkyl, cycloalkyl, alkylaryl and cycloalkylaryl esters of phosphoric acid have become known. The anti-static However, the effectiveness of these compounds is not sufficient.

A group of surface-active substances that have so far not played a major role in practice, is that of the ampholytes, generally obtained by reaction between compounds with positive groups, such as Amino, ammonium or pyridine groups, and compounds with negative groups, such as carboxyl, sulfo- or phosphoric acid groups.

It has now been found that for antistatic finishing of polyethylene terephthalate threads or fibers, reaction products which by reaction of Polyäthyleneglykolen with Metaphosphorsäurealkylestern and subsequent reaction with alkyl or alkylolamines

, 0R

= P,

Procedure for antistatic finishing

of polyethylene terephthalate threads

or fibers

Applicant:

United Glanzstoff-Fabriken AG,
Wuppertal-Elberfeld, Am Laurentiusplatz

Dr. Karl Macura, Klingenberg / M.,

and Dr. Erhard Siggel, Laudenbach / M.,

have been named as inventors

arise, are particularly well suited. These avivage agents are used in the form of solutions brought.

The starting products of the compounds to be used as softeners according to the invention, namely the Metaphosphoric acid alkyl esters can be prepared according to the procedures described in the literature:

1. by heating lower alkyl ethers with P ₂ O ₅ ,

2. by thermal decomposition of dialkyl chlorophosphate,

3. by thermal decomposition of tetraalkyl phosphates into trialkyl phosphate and alkyl meta-phosphate,

4. by reacting trialkyl phosphates with P ₂ O ₆ . Of the alkyl metaphosphoric acid esters which can be obtained in accordance with these reactions, the ethyl metaphosphoric acid ester, which is obtained in the reaction of diethyl ether with P ₂ O _5, is particularly suitable for the preparation of antistatic softeners.

The implementation of the phosphoric acid alkyl ester with polyglycols takes place according to the following equation:

+ HO- (CH ₂ -CH ₂ O) ₁₁ -H ^ O

OR

= P ^ O- (CH ₂ -CH ₂ -O) _x H
OH

wherein polyglycols with molecular weights from 200 to 45 with an alkyl or alkylolamine, e.g. B. stearyl or 1000 can be used. The poly cetylamine obtained, further reacted:
Ethylene glycol-alkyl-phosphoric acid ester is then

OR, OR

O = P ^ -O- (CH ₂ -CH ₂ O) _x H + H ₂ NR 'OH

= P

CH ₂ -O) _x H

Depending on the choice of polyglycols, products with a semi-solid to waxy consistency are obtained, which in water and Ο - (CH ₂ - ^X OH ^ N ⁺ R '

are soluble in most organic solvents. They can be used as a softener or spin finish

009 54S / 417

Find use. Treating the threads and fibers with these softeners guarantees a good one Processability, e.g. B. on cards or carding machines, in particular reducing the electrostatic charge plays an essential role.

The process according to the invention is explained in detail by means of examples and a known one Softeners compared.

example 1

In a mixture of polyethylene glycols of molecular weight 200 and 300 (weight ratio 1: 1.5) equimolecular amounts of Metaphosphorsäureäthylester under stirring at 4O ⁰ C was slowly added. The resulting reaction mixture is then heated at 85 to 90 ° C. for about 6 to 8 hours. The obtained highly viscous Polyäthylenglykoläthylphosphorsäureester which was dissolved in water has a _pH value of 1.5 is added then an equimolar amount of molten stearylamine stirring well. Are both Kornponenten mixed properly, obtained after cooling a homogeneous Avivagepaste with a solidification point of 46 ° C and a _pH value of 7.1 in L ° / _o aqueous solution. The reaction product is readily soluble in water, benzene, alcohol and petroleum ether. It becomes a 0.18 ° / ₀ aqueous lubricant-containing bath (bath ratio 1: 20) were recognized. With this liquor polyethylene terephthalate fibers are brightened by 15 minutes immersion at 60 to 65 ⁰ C. The fibers are then spun off in the centrifuge to a moisture content of 10% and ^{dried at 100 °} C., ^{conditioned and carded at 24 °} C. and 60% relative humidity for 24 hours. The carding is carried out on a card with all-steel clothing without a flounce with a top hook clothing. This gives a charge of -260 volts. (The charging is measured with a field mill device.)

Example 2

In Metaphosphorsäureäthylester equimolecular amounts of polyethylene glycol are added to the molecular weight 600 at about 50 to 6O ⁰ C slowly with stirring, heated for a further 4 to 6 hours at 80 to 90 ° C and then fused with equimolecular amounts of triethanolamine at 60 to 70 ⁰ C. The paste-like product obtained, which is also soluble in water and in most organic solvents, is used according to Example 1 as a softener for polyethylene terephthalate fibers. When treated and measured under the conditions described in Example 1, an electrostatic charge of -150 volts *. established. ■ ",. -.:.

The mentioned in the introduction organophosphate-alkylene oxide adducts loan, as the following \ ^r ergleichsbeispiel shows the polyethylene terephthalate fibers not have nearly the same antistatic properties.

Comparative example

A nonionic ethoxylated alkylene phosphoric acid ester, which is obtained by reacting 1 mole of phosphorus pentoxide with 2 moles of cetyl alcohol and 4 to 5 moles of ethylene oxide (corresponding to a molecular weight of about 200) with heating to 100 to 150 ^° C., is used as described in Example 1, to a 0.18 ° / ₀ by weight of lubricant-containing bath. When polyethylene terephthalate fibers are treated with this liquor under otherwise identical conditions, a charge of -1500 volts is measured.

It is a known fact of experience that when carding polyethylene terephthalate fibers, the level of charge of the fleece should not exceed a value of - 1000 volts, as a security with regard to the Otherwise, preservation of the anti-static effectiveness during further textile processing of the fibers cannot be guaranteed.

If you want a charge level of the fleece below -1000 volts even with less effective antistatic Achieve funds, this can only be done with more concentrated avivage fiotten. Through the higher application of the antistatic agent on the fiber surface in the form of a thick film of grease, however, there is then the risk of so-called smearing on the Card.

The softeners according to the invention offer the advantage over the compound described in the comparative example that they are very effective even in very low concentrations. In addition, they have a much better thermal stability, so that no disadvantages in the textile processing, z. B. in finishing processes that are carried out at higher temperatures occur. Even with hot air treatment at 210 ^° C. for up to one hour, there are no signs of yellowing, nor is the antistatic effectiveness noticeably reduced. In contrast, the finishing agent of Comparative Example decompose already at 110 ⁰ C with gas evolution.

Claims (1)

Claim: Process for the antistatic softening of polyethylene terephthalate threads or fibers using organic phosphorus compounds, characterized in that the softening agents used are the reaction products which are formed by reacting polyethylene glycols with alkyl metaphosphoric acid esters and then reacting with alkyl or alkylolamines. Considered publications:
British Patent No. 769 039. 009 548/417 6.60