EP0022239B1 - Agent and process for wet paraffinic treatment of yarns - Google Patents

Description

In order to be able to use dyed or undyed staple fiber yarns for knitting, it is common to treat them with a solid paraffin block during a rewinding process. A certain amount of solid paraffin is applied to the fiber and receives the low coefficient of friction required for the further processing process, i.e. a high smoothness. It is understandable that this process of so-called dry waxing is not without problems in practice. Depending on the pressure between the fiber and the paraffin block, the amount of dry paraffin may fluctuate. The solid paraffin can sublime away in subsequent heating processes (ironing, fixing) and thus tend to bloom. The rigid dry paraffin gives the material sufficient smoothness for further processing, but there is no actual softening effect associated with its application. There is therefore a need for dry-waxed articles to soften these articles in a subsequent work step by applying an additional plasticizer.

Furthermore, the preparation of fibers with aqueous wax emulsions is known from DE-AS No. 1239057. FR-A No. 2322963 describes the use of hydroxyalkylimidazoles esterified with fatty acids as fabric softeners. The use of amine oxides as antistatic agents for fibers is known from FR-A No. 2230790.

• a) 5-20% Paraffin, Schmelzbereich 45-60° C;
• b) 2-10% eines oder mehrerer Alkylimidazoline der Formel
  
  wobei
  • R C₁₂-C₂₂-Alkyl, Alkenyl oder Hydroxyalkyl,
  • R, Wasserstoff oder C₁-C₂₂-gesättigtes oder ungesättigtes aliphatisches oder aromatisches Acyl,
  • R₂ Wasserstoff, C, -C4-Alkyl oder Hydroxyalkyl,
  • n Zahlen von 2-6, und
  • X ein Halogen-, C,-C₄-Alkylsulfat-, C,-C₄-Dialkylphosphat- oder ein C,-C₄-Alkylcar- boxylatanion bedeuten;
• c) 1-5% eines oder mehrerer Aminoxide der allgemeinen Formel
  
  wobei
  • R C₈-C₁₈-Alkyl oder Alkenyl,
  • R, C,-C4-Alkyl,
  • R2 Wasserstoff oder C, -C₄-Alkyl, und
  • n Zahlen von 0 bis 6 bedeuten;
• d) 5-20% eines oder mehrerer Polyglykoläther der Formel
  
  wobei:
  • R C₈-C₁₈-Alkyl oder Alkenyl und
  • n Zahlen von 3 bis 12 bedeuten, und
• e) der an 100 Gew.% fehlende Rest ist Wasser.

It is therefore the task of giving staple fiber yarns a uniformly low friction which is necessary for further processing, ie high smoothness combined with satisfactory softness. The object is achieved by using a liquid paraffin waxing agent with the following composition:

• a) 5-20% paraffin, melting range 45-60 ° C;
• b) 2-10% of one or more alkylimidazolines of the formula
  
  in which
  • RC ₁₂ -C ₂₂ alkyl, alkenyl or hydroxyalkyl,
  • R, hydrogen or C ₁ -C ₂₂ -saturated or unsaturated aliphatic or aromatic acyl,
  • R _{2 is} hydrogen, C, -C4-alkyl or hydroxyalkyl,
  • n numbers from 2-6, and
  • X is a halogen, C, -C ₄ -alkyl sulfate, C, -C ₄ -dialkyl phosphate or a C, -C ₄ -alkylcarboxylate anion;
• c) 1-5% of one or more amine oxides of the general formula
  
  in which
  • RC ₈ -C ₁₈ alkyl or alkenyl,
  • R, C, -C4 alkyl,
  • R2 is hydrogen or C, -C ₄ alkyl, and
  • n is a number from 0 to 6;
• d) 5-20% of one or more polyglycol ethers of the formula
  
  in which:
  • RC ₈ -C ₁₈ alkyl or alkenyl and
  • n are numbers from 3 to 12, and
• e) the rest missing from 100% by weight is water.

• 8-12% Paraffin (Fp. 50-53° C),
• 3- 6% eines Imidazolins der Formel I, wobei
  • R C₁₂-C₁₈-Alkyl,
  • R, C₁₆-C₂₂-Acyl,
  • R₂ Wasserstoff,
  • X- Cl- oder CH₃COO―, und
  • n 2 oder 3 bedeuten,
  • 3-5% eines Aminoxids der Formel II, wobei
  • R C₈-C₁₂-Alkyl oder Alkenyl,
  • R, und R₂ Methyl, und
  • n 0 bedeuten,
• 6-10% eines Polyglykoläthers der Formel III, wobei
  • R kokosalkyl (C₁₂-C₁₈-Alkyl und Alkenyl),
  • n Zahlen von 4 bis 8 bedeuten,
  • und der an 100 Gew.% fehlende Rest ist Wasser.

An agent of the following composition is preferably used:

• 8-12% paraffin (mp 50-53 ° C),
• 3- 6% of an imidazoline of the formula I, where
  • RC ₁₂ -C ₁₈ alkyl,
  • R, C ₁₆ -C ₂₂ acyl,
  • R _{2 is} hydrogen,
  • X- Cl- or CH ₃ COO―, and
  • n is 2 or 3,
  • 3-5% of an amine oxide of formula II, wherein
  • RC ₈ -C ₁₂ alkyl or alkenyl,
  • R, and R _{2 are} methyl, and
  • n means 0
• 6-10% of a polyglycol ether of the formula III, where
  • R cocoalkyl (C ₁₂ -C ₁₈ alkyl and alkenyl),
  • n are numbers from 4 to 8,
  • and the rest missing from 100% by weight is water.

The paraffin dispersion is produced by intensive mixing of all components at temperatures of over 70-80 ° C., a particular advantage being that no homogenizer is required.

The clear dispersions are stable and can be diluted with cold water to the desired final concentration in an aqueous liquor. These paraffin dispersions, which form fine and stable shear dispersions when diluted with water, can be used instead of solid dry paraffin to wax staple fiber yarns from native and synthetic fibers. They can be called pseudo-cationically dispersed systems and are characterized by high substantivity when used in a long fleet. The pH value of the paraffin dispersions is advantageously 3-6 when used and is adjusted to this value with acids.

The paraffin dispersions are applied in customary dyeing machines such as those used for dyeing textile yarns. We work in fleet ratios from 1: 5 to 1:40 at temperatures of 10-90 ° C. The application is advantageously carried out after the dyeing process, by treating the yarn after rinsing with a dispersion of the type described above in a dilute aqueous form which contains 0.1-2% by weight, preferably 0.3-1% by weight of the composition of the composition described above, based on the weight of the yarn.

In addition to the desired smoothness, the yarns paraffinized in this way have a pleasantly soft feel, which makes the application of an additional plasticizer unnecessary. Due to the dispersing agents built into the systems, there is no electrostatic charge interfering with knitting. The paraffin dispersions according to the invention also do not contain any organic solvents which could be harmful to the environment, especially when working in open apparatus. They only contain the inexpensive paraffin as a sliding component and do not require any additional components for conveying smoothness and the softening effect, e.g. Fatty acid esters, which are expensive compared to paraffin. The paraffin dispersions according to the invention have a high substantivity, combined with a high wetting power, which enables application even in short test times and at a low temperature.

The dispersions according to the invention give yarns a high antistatic effect combined with high smoothness.

The dispersions described in the following examples are prepared by simply mixing the individual components. Percentages are to be understood as% by weight. EO means ethylene oxide.

example 1

• 15 Teile Paraffin (Fp. 50-53° C),
• 5 Teile eines Imidazolins der Formel I, wobei
  • R ein Gemisch aus 45% C₁₅- und 55% C₁₇-Alkyl,
  • R, ein Gemisch aus 45% C₁₆- und 55% C₁₈-Acyl,
  • R₂ Wasserstoff,
  • n 2
  • X― CH₃CO₂― bedeutet,
• 4 Teile kokosalkyldimethylaminoxid,
• 10 Teile kokosfettalkohol x 5 EO
• 100 Teile elektrolytfreies Wasser (E-Wasser). pH-Wert: ca. 4.

Paraffin dispersion consisting of

• 15 parts paraffin (mp 50-53 ° C),
• 5 parts of an imidazoline of the formula I, where
  • R is a mixture of 45% C ₁₅ and 55% C ₁₇ alkyl,
  • R, a mixture of 45% C ₁₆ and 55% C ₁₈ acyl,
  • R _{2 is} hydrogen,
  • n 2
  • X― CH ₃ CO ₂ - means
• 4 parts of cocoalkyldimethylamine oxide,
• 10 parts coconut alcohol x 5 EO
• 100 parts of electrolyte-free water (E-water). pH value: approx. 4.

Example 2

• 17 Teile Paraffin (Fp. 50-53° C),
• 7 Teile des Imidazolins nach Beispiel 1,
• 4 Teile Oleyldiethylaminoxid,
• 8 Teile Oleylalkohol x 7 EO,
• 100 Teile E-Wasser.
• pH-Wert: ca. 4,2.

Paraffin dispersion consisting of

• 17 parts paraffin (mp 50-53 ° C),
• 7 parts of the imidazoline according to Example 1,
• 4 parts of oleyldiethylamine oxide,
• 8 parts oleyl alcohol x 7 EO,
• 100 parts of demineralized water.
• pH: approx.4.2.

Example 3

• 13 Teile Paraffin (Fp. 52-54° C),
• 6 Teile eines Imidazolins der Formel I, wobei
  • R ein Gemisch aus 5% C₁₃-, 30% C₁₅-, 35% C₁₇-Alkyl und 30% C₁₇-Alkenyl,
  • R, ein Gemisch aus 5% C₁₄-, 30% C₁₆-, 35% C₁₈-Acyl und 30% C₁₈-Acenyl,
  • R₂ Wasserstoff,
  • n 2, und
  • X- Acetat- bedeutet,
• 3 Teile eines Aminoxids der Formel II wobei
  • R ein Gemisch aus 70% C₁₂- und 30% C₁₄-Alkyl,
  • R, und R₂ Methyl, und
  • n 0 bedeutet und
• 6 Teile kokosfettalkohol x 6 EO,
• 6 Teile Oleylalkohol x 5 EO,
• 100 Teile E-Wasser. pH-Wert: 4,5.

Paraffin dispersion consisting of

• 13 parts paraffin (mp 52-54 ° C),
• 6 parts of an imidazoline of the formula I, where
  • R is a mixture of 5% C ₁₃ -, 30% C ₁₅ -, 35% C ₁₇ -alkyl and 30% C ₁₇ -alkenyl,
  • R, a mixture of 5% C ₁₄ -, 30% C ₁₆ -, 35% C ₁₈ -acyl and 30% C ₁₈ -acenyl,
  • R _{2 is} hydrogen,
  • n 2, and
  • X- acetate- means
• 3 parts of an amine oxide of formula II wherein
  • R is a mixture of 70% C ₁₂ and 30% C ₁₄ alkyl,
  • R, and R _{2 are} methyl, and
  • n means 0 and
• 6 parts coconut alcohol x 6 EO,
• 6 parts oleyl alcohol x 5 EO,
• 100 parts of demineralized water. pH: 4.5.

Example 4

• 14 Teile Paraffin (Fp. 52-54° C),
• 2,4 Teile des in Beispiel 1 verwendeten Imidazolins,
• 0,6 Teile eines Imidazolins der Formel wobei
  • R ein Gemisch aus 5% C,_a-, 30% C₁₅-, 35% C₁₇-Alkyl und 30% C₁₇-Alkenyl,
  • R, und R₂ Wasserstoff,
  • n 2, und
  • X― CH₃COO― bedeutet,
• 6 Teile kokosalkyldimethylaminoxid, und
• 10 Teile C₁₂/C₁₄-Alkohol _x 10 EO,
• 100 Teile E-Wasser. pH-Wert: 4,1.

Paraffin dispersion consisting of

• 14 parts paraffin (mp 52-54 ° C),
• 2.4 parts of the imidazoline used in Example 1,
• 0.6 parts of an imidazoline of the formula wherein
  • R is a mixture of 5% C, _a , 30% C ₁₅ , 35% C ₁₇ alkyl and 30% C ₁₇ alkenyl,
  • R, and R _{2 are} hydrogen,
  • n 2, and
  • X― CH ₃ COO― means
• 6 parts of cocoalkyldimethylamine oxide, and
• 10 parts of C ₁₂ / C ₁₄ alcohol _x 10 EO,
• 100 parts of demineralized water. pH: 4.1.

Example 5

Yarns made of 100% polyester (PES), after previous dispersion dyeing and rinsing at 40 ° C. for 30 minutes in a liquor ratio of 1:10 at pH 5.5, were diluted in a cross-winder dyeing apparatus under cooking temperature conditions treated. These dispersions were diluted to such an extent that the concentration of components a) to d) in the liquor, based on the weight of the yarn, was 2% by weight. After drying, the PES material had a smooth, soft feel, which can only be achieved with dry-paraffinised yarns with the addition of a cationic softener.

The wet waxed yarns are very smooth. The coefficient of friction, measured in the measuring arrangement described in DE-A No. 2416430, gave the following values at the measuring speeds 20 and 100 m / min:

The material was easy to process and showed a uniform, homogeneous surface after being knitted.

The following antistatic values in meg-ohms at 22 ° C and 65% r. F. measured:

Similar favorable effects are achieved if instead of PES yarns, wool yarns, cotton yarns or polyacrylonitrile yarns or blends are used.

Claims (3)

1. Agent for the wet paraffin waxing of yarns on the basis of paraffin which consists of:

a) from 5 to 20% of paraffin, melting range of 45 to 60° C;

b) from 2 to 10% of one or several alkyl imidazolines of the formula:

in which:

R is alkyl, alkenyl or hydroxyalkyl, each with 12 to 22 carbon atoms,

R₁ is hydrogen or C₁-C₂₂-saturated or unsaturated aliphatic or aromatic acyl,

R₂ is hydrogen, C₁-C₄-alkyl ou C₁-C₄-hydroxyalkyl,

n is a number of from 2 to 6, and

X is a halogen anion, a C, -C₄-alkyl sulfate anion, a C₁-C₄-dialkyl phosphate anion, or a C₁-C₄-alkylcarboxylate anion,

c) from 1 to 5% of one or several aminoxides of the general formula:

in which:

R is C₈-C₁₈-alkyl or alkenyl,

R, is C₁-C₄-alkyl, and

R₂ is hydrogen or C₁-C₄-alkyl, and

n is a number of from 0 to 6, and

d) from 5 to 20% of one or several polyglycol others of the formula:

in which:

R is C₈-C₁₈-alkyl or alkenyl, and

n is a number of from 3 to 12, as well as water ad 100%.

2. Agent as claimed in claim 1 which consists of:

from 8 to 12% of paraffin (m.p. 50-54° C),

from 3to 6% of an imidazoline of formula (I), in which:

R is C₁₂-C₁₈-alkyl,

R, is C₁₆-C₂₂-acyl,

R₂ is hydrogen,

X- is Cl― or CH₃COO―, and

n is 2 or 3,

from 3 to 5% of an aminoxide of formula (II), in which:

R is C₈-C₁₂-alkyl or alkenyl,

R, and R₂ are methyl, and

n is 0,

from 6 to 10% of a polyglycol ether of formula (III), in which:

R is C₁₂-C₁₈-alkyl and alkenyl (coconut oil alkyl), and

n is a number of from 4 to 8,

and water ad 100%.

3. Process for the wet paraffin waxing of native and synthetic yarns, which comprises treating the yarns according to the batchwise exhaustion method at a pH of 3 to 6, a goods-to-liquor ratio of from 1 : 5 to 1: 40, and a temperature of from 10 to 90° C, with an agent as claimed in claim 1 or 2.