DE1719355A1 - Process for the optical brightening of fiber materials made of synthetic polyamides or cellulose esters - Google Patents

Description

for patent application Fw 5654

Process for the optical brightening of fiber materials ^

made of synthetic polyamides or cellulose esters

It is known that synthetic fiber materials made of linear polyesters can be produced using the so-called thermosol process, d. H. by padding at room temperature with solutions or suspensions of suitable, water-insoluble ones optical brighteners and subsequent heat treatment can optically brighten with good success. the Heat treatment to fix the brighteners is preferred carried out at temperatures at which a thermal stabilization of the pulp is carried out at the same time

he follows. These are for polyester fibers generally ä

Temperatures between about 170 and 220 C.

Attempts have also been made to treat fiber materials made of synthetic polyamides by the thermosol process, but The effects that can be achieved with optical brighteners are far worse than those that can be achieved with the otherwise usual Exhaust process can be obtained. That is why the thermal insulation failed optical brighteners on polyamide fibers have so far not gained any significance.

109832/163?

In principle, the same difficulties arise with the optical brightening of fiber materials made of cellulose esters, especially made of cellulose triacetate, after the thermosol process on.

It has now been found that it is possible to avoid these difficulties and to use fiber materials as synthetic Polyamides or cellulose esters after the thermosol process lighten with good success if one uses a mixture of a polyalkylene glycol as an aid and an oxethylated fatty alcohol is used.

The present invention thus provides a method for the optical brightening of fiber materials made of synthetic polyamides or cellulose esters by impregnation with a liquor containing optical brighteners and subsequent fixing of the optical brighteners by heat treatment, the fixing in the presence of an auxiliary mixture of polyalkylene glycol with about 2 to 22 of the units - (CH ₀ O) -, in which η 2 or

η 2η

means, and an oxethylated fatty alcohol with one Alkyl radical of at least 8 carbon atoms and about 3 to 16 ethylene glycol ether units in the molecule.

Those to be used according to the invention are expedient Auxiliary mixture also added foam-suppressing products. As such, for example Consider 'aliphatic carboxylic acid esters of the formula

R ₁ - 0 - C - R ₂ , 0

where! I. unu? < _v same or different »· !, saturated

1 0 98 3 2/1 6 3 7

I / I

or are unsaturated alkyl groups each having 4 to 18 carbon atoms, one or both of which have at least one side chain, preferably in the 2-position. Suitable esters of this type are, for. B .: 2-Xthylhexyl-2- & thylcaproic acid ester, 2-Xthylbutyl-2-ethylcaproic acid ester, 2-ethylhexyl-dimethyl-isopropyl acetate, isooctyl-2-ethylcaproic acid ester, isobutyl-2-ethylcaproic acid ester with the 2,6-caproic acid ester , 8-Trimethylnonanol- (4) and the 2-ethylcaproic acid ester of 2,6-dimethylheptanol ~ (4>. The carboxylic acid esters are preferably mixed together with a phosphoric acid ester of an aliphatic alcohol with 4 to 8 carbon atoms, e.g. triisobutyl phosphate The foam-suppressing substances are generally added to the auxiliary mixture to be used according to the invention in amounts of 0.5 to 5 % each, based on the weight of the auxiliary mixture.

The method according to the invention can be carried out by adding a solution or emulsion containing the optical brightening agent and the polyalkylene glycol, the oxethylated fatty alcohol and optionally other auxiliaries contains, applies to the fiber material to be lightened, this pre-dries and in a thermosol system a Subjected to heat treatment and then finished in the usual way. The optical brightening agents can be applied from organic or preferably aqueous liquors. It is also possible to use the optical brightening agents on the one hand and those used according to the invention Auxiliaries and optionally the foam suppressants on the other hand in any order one after the other to apply the heat treatment to the fiber material.

109832/1637

The heat treatment for fixing the optical brightening agents is generally carried out at temperatures of about 170 ° to 220 ° C, preferably 180 ° to 210 ° C, for about 5 to 60, preferably 5 to 40 seconds, carried out as dry heating, if necessary with the introduction of some steam.

As polyalkylene glycols to be used according to the invention come compounds of the general formula

^H0 - ^(C n ^H 2n °> x ^H

where η is 2 or 3 and χ is a value between about 2 and 22 means under consideration. Polyethylene glycols with an average molecular weight preferably come between 200 and 600 are used. However, poly » propylene glycols or polyethylene propylene glycols as well Find mixtures of polypropylene glycols and polyethylene glycols use.

Compounds of the formula come as oxäthyUerte fatty alcohols

RO- (CH ₂ -CH ₂ -O) ₂₁ H,

wherein ζ values from about 3 to 16, preferably 5 to 10, and R is a saturated or unsaturated alkyl radical is at least β, preferably 12 to 18, carbon atoms, for use.

The mixing ratio between the polyalkylene glycols and the oxäthyllerten fatty alcohols can be used within wide limits

./ 109832/1637

ί7Ϊ'935Β

tllt ** eini ier * «n on .in dMriefttltiii der

έί ** O, 01 to 1 düicatiteil, tor.of * - $ yS G * VichtSteile, the oxtthylated fettilkOholi ftitt ^ indt. The length of the application

bfctrift _z ** cioitöii ettaV _v Ö5 -bi «J, 5% to 1.5%, based on the dish of the

Approaches to the present invention are known to those skilled in the art

D- and ceilulose acetate fiber materials are suitable for use in whitening agents. Preferably Lightening agent from the series of pyrazoline compounds, those of the old formula

Ä »-

ent speaking, burned. In the formula, R 'means one li A substituted aryl radical and X is a vinyl

group or a radical -CH ₃ -CH ₂ -T, in which T is a hydroxyl group, an -OSCt ₅ Ae or a -SO «Me group and in which ie for hydrogen, a metal cation or a primary or secondary alino group, an acyl aino group or an optionally substituted alkoxy radical. Such optical brightening agents are described, for example, in Belgian patents 631,367, 381,139, 670,161 and 701,986. For use on fiber materials made of synthetic polyamides, water-soluble brightening agents of the type mentioned are mainly used,

The lightening agents are used in the usual use concentrations. In general, quantities

109832/1637 './.

IT? 19355

-B-

of about 0.01 bli 3 l based on the weight of the fiber material.

The inventive method can be applied to fiber materials made of synthetic polyamides, e.g. B. those au * adipic acid and HexaeethylendiaS-in (polyamide 66) from adipic acid, Kexa- »Ethylenediamine and caprolactam (polyamide 66/6), from caprolactam (polyamide 6) or from n-aminoundecylic acid (polyamide 11), as well as on fiber materials made from cellulose esters, in particular cellulose triacetate, can be used.

According to the method according to the invention, goods with a uniformly high whiteness obtained.

1098 3 2/1637

ORIGINAL INSPECTED

Example I.

A knitted fabric made of polycaprolactam (polyamide 6) is impregnated with a liquor containing ₍ 15 g / l of an auxiliary ■ ischung consisting of 85 parts of polyethylene glycol with a molecular weight of 400, 10 parts of an adduct of 5 moles of ethylene oxide _with 1 mole of C ₁₃ fatty alcohol , 2.5 parts of triisobutyl phosphate and 2.5 parts of 2-ethylcaproic acid 2-ethylbutyl ester, 15 g / l of an optical brightening agent of the formula

and contains 0.3 g / l citric acid.

The textile material is squeezed between rollers until it still contains 70 % of its dry weight in liquid and then hot air treatment for 20 seconds

Exposed to 190 ° C. j f

■ {

The knitted fabric treated in this way has an excellent degree of whiteness, j

which is much closer than that which aan is otherwise equal to ί chen conditions, but without using the auxiliary means, j receives.

Example 2 A washed and dried fabric made of polyamide 6.6

109832/1637

is treated with a liquor containing 25 g / l of an auxiliary agent mixture consisting of 75 parts of polypropylene glycol with a molecular weight of 250, 15 parts of an adduct of 8 parts of ethylene oxide with 1 mole of iso-C ₁₃ fatty alcohol, 5 parts of triisobutylphosphate and 5 parts 2-ethyl-caproic acid-2-ethylbutyl ester, 25 g / l of an optical brightening agent of the constitution listed in Example 1 and 0.5 g / l citric acid. In addition, 30 g / l of the dye CI No. 51 319 see Color Index 2nd edition (1956) are added to the liquor to correct the shade of the brightener.

The textile material is squeezed between rollers in the usual way until it still contains 55 % of its dry weight in liquid. It is then dried at 130 ° C. for 30 seconds and then subjected to hot air treatment at 200 ° C. for 20 seconds.

The knitted fabric treated in this way has an excellent degree of whiteness, which is considerably higher than that which is otherwise equal Conditions, but without auxiliary equipment, is obtained.

Example 3

A knitted fabric made of polyamide 6 is treated with a liquor containing 25 g / l of an auxiliary mixture consisting of 85 parts Polyethylene glycol of molecular weight 200, IO parts of one Addition product of 5 moles of ethylene oxide and 1 mole Stearyl alcohol, 2.5 parts triisobutylphoephate and 2.5 parts 2-ethylcaproic acid-2-ethylbutyl ester, 5.7 g / l deseptic Brightening means of the formula

109832/1637

γ * ^ NH ^ V CH-

ft ^

contains.

You «textile material is squeezed between rollers, bia es BOcb contains SO% of its dry weight «in liquid followed by 20 seconds of hot air treatment

exposed to 190 ° C.

The knitted fabric treated in this way has a very high degree of whiteness.

Example 4

Sin 'fabric made of triacetate fiber is impregnated with a liquor. alert, the 20 g / l of an auxiliary mixture of the composition in Example 1, 2.25 g / l of an optical brightening agent of the formula

SOj-CHj- (JB ₃ -

r Aeltfertmgsverbiadua | rm 8 mol Xtnylenaxiden ^v thAl D Ttilt id l ^

| G

«« Noel)! (Γ * of his TrookengewiOltes X W4 t »« «hii« «end 10 seconds

will

Example 5

BiB knitted fabric made of polyamide ~ 6 was treated with a liquor the 2Ä g / l of an aid «, consisting of 85 parts Polyethylene glycol with a molecular weight of 200, 10 parts of an adduct of 5 moles of ethylene oxide and 1 mole of oleyl alcohol, 2.5 parts of triisobutyl phosphate and 2.5 parts of 2-xthyloaproic acid 2-ethylbutyl ester, 5.7 g / l of an optical Aufheilungealt means of the constitution listed in Example 1 and 0.5 contains g / l citric acid. The textile material wetted in this way is squeezed off by rollers until it is only 50% of its size Dry weight of liquid contains and adjoining Subjected to hot air treatment at 190 ° C for 20 seconds.

The knitted fabric treated in this way has an excellent degree of whiteness.

109832/1637

ORlGlNAL

• Ά

Claims (3)

- li - claims 1. A process for the optical brightening of fiber materials made of synthetic polyamides or cellulose esters by impregnation with a liquor containing a brightening agent and subsequent fixing of the optical brighteners by heat treatment, characterized in that the brightening agent is fixed in the presence of an auxiliary mixture of polyalkylene glycol containing about 2 to 21 of the units - (C _n Ha _n ⁰ ) - »where η is 2 or 3, and an oxithylated fatty alcohol with an alkyl radical of at least 8 carbon atoms and about 3 to 16 ethylene glycol ether units in the molecule. 2. The method according to claim I _1, characterized in that, together with the auxiliary mixture, small amounts of a Phosphorstureestera aliphatic alcohols having 4 to 8 carbon atoms and a carboxylic acid ester of the formula in which R and R ₂ , identical or different types of saturated> or unsaturated alkyl groups of 4 to 18 carbon! Substance atoms mean at least one branch of which has 1 to 4 carbon atoms, preferably in the 2-position, are used as foam-suppressing agents. 3. The method according to claim 1 or 2, characterized in that that the auxiliaries are applied to the fiber materials together with the optical brightening agents. 109832/163?