JPH02259173A - Mixture of auxilialies and use thereof in dyeing of polyester fiber material - Google Patents

Abstract

PURPOSE: To obtain an auxiliary mixture comprising a specific dicarboxyimide ester, an acidic ester and a nonionic surfactant, capable of improving migrating properties of a dye, manifesting excellent level dyeing effects and assuring good fastness by adding thereof to a dye bath of a disperse dye. CONSTITUTION: This auxiliary mixture is obtained by compounding (A) 20-70 wt.% (based on the total mixture) of a dicarboxyimide ester represented by formula I [W is a >=2C dicarboxylate group; R is a <=24C aliphatic group, a <=24C araliphatic group or a <=24C cycloaliphatic group; (n) is 2-25] with (B) 15-40 wt.% (based on the total mixture) of an acidic ester of an alkylene oxide adduct represented by formula II [V is H or CH3 ; X is an inorganic or an organic acid group containing oxygen; Y is an α-methylaralkyl; the alkylene is ethylene or propylene; (m) is 1-3; m1 is 1 or 2; n2 is 4-50] or its salt and (C) 15-40 wt.% (based on the total mixture) of a nonionic surfactant. The auxiliary mixture is made to coexist in an amount of 0.3-6 g/L in a dye bath of a disperse dye to dye polyester fibers. The migrating properties of the dye are promoted to afford level dyeing effects.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to novel mixtures of auxiliaries and their use in the dyeing of polyester fiber materials.

The auxiliary mixture according to the invention contains at least the following three components: (A) of the formula (wherein W is the residue of a dicarboxylic acid having at least 2 carbon atoms; R is not more than 24; Aliphatic radicals, preferably having not more than 12 carbon atoms, araliphatic (araliphatic)
iphatic) group or cycloaliphatic group, n is 2 to 25), a dicarboximide ester of the formula (B) (wherein ■ is hydrogen or methyl, and X is an oxygen-containing inorganic acid, such as sulfuric acid) or phosphoric acid, an acid group or a residue of an organic acid, Y is an α-methylaralkyl group, alkylene is an ethylene or propylene group, m is 1 to 3, m is 1 or 2, and R2 is 4 to 50. ) or a salt thereof; (C) a nonionic surfactant preferably containing a polyethylene glycol ether group;

The auxiliary mixture according to the invention advantageously contains, based on the total mixture, 20 to 70% by weight of component (A), 15 to 40% by weight of component (B), and 15 to 40% by weight of component (C). %contains.

Components (A), (B), (C) may be present as a single compound or as a mixture of two or more compounds.

Components (B) and (C) are preferably used as a mixture.

W in formula (1) is, for example, a divalent aliphatic, cycloaliphatic or aromatic group, and is bonded to the carboxyl group of the imide group.

If W is a divalent aliphatic group, it is preferably an unsubstituted or halogen-substituted linear or branched saturated or ethylenically unsaturated dicarboxylic acid having from 4 to 10 carbon atoms (PJ). It is a branched hydrocarbon group. Examples of suitable aliphatic saturated dicarboxylic acids of this type are succinic acid and glutaric acid. Preferred examples of ethylenically unsaturated dicarboxylic acids are maleic acid, dimethylmaleic acid. acids, dichloromaleic acid, citraconic acid, cultaric acid, and itacone.

When W is a divalent cycloaliphatic group, it is especially
It is a residue of lahydrophthalic acid or hexahydrophthalic acid.

If W is a divalent aromatic dicarboxylic acid group, it is for example the residue of naphthalene dicarboxylic acid or phthalic acid.

Preferably W is a phenylene group which may be substituted by halogen such as chlorine, bromine, C+ C4-alkyl such as methyl or tert-methyl, or C+ C-alkoxy such as methoxy. Particularly preferably W is an unsubstituted phenylene group.

The aliphatic group R can be saturated or unsaturated, linear or branched. Preferably, R is an argyl radical having 1 to 24, particularly preferably 1 to 12 carbon atoms. Examples of such alkyl groups include methyl, ethyl, n-propyl, isopropyl, n-methyl, 5ec-
Methyl, pentyl, n-hexyl, 2-ethylhexyl, 1.1.3.3 tetramethyl, n-octyl, n
-1": tecyl, myristyl, ophtatcyl, araxyl, behenyl. Examples of cycloaliphatic radicals R are cyclopentyl or especially cyclohexyl. Particularly preferred examples of R as araliphatic radicals are hensyl radicals. be.

n is preferably 5.

The industrially important dicarboximide ester of formula (1) is represented by the following formula.

where W is alkylene or alkenylene having 2 to 4 carbon atoms, cyclohexylene, or phenylene unsubstituted or substituted by a halogen such as chlorine or bromine, methyl or methoxy;
R1 is alkyl having 1 to 12, preferably 3 to 8 carbon atoms, cyclohexyl or pencil.

,4. :Cicalboximine 1-' used according to the invention
Representative examples of esters are shown below.

Methylphthalimide 1-'hexanoate, ethyl phthalimide 1-hexanoate, propyl phthalimide hexanoate, n-phthalimide hexanoate, 2
-Ethylhexyl phthalimidohexanoate, n-phthylhexahydrophthalimidohexanoate, 2-ethylhexylhexylhexanoate, n-phthyltetrahydrophthalimidohexanoate, n-butyltetra Chlorophthalimidohexanoate, 2-ethylhexyltetrachlorophthalimidohexanoate, n-phthylsuccinimitohexanoate, 2-ethylhexylna-1-rahitophthalimidohexanoate.

Among these representative examples, preference is given to C5-08-alkyl phthalimidohexanoe-1, especially to 03Co-alkylphthalimide hexanoe-1, such as 2-ethylhexylphthalimide-hexanoe-1.

The compounds of formulas (1) and (3) are produced by methods known per se. The preferred cyclophonic anhydride is
It can be carried out by reacting a Ni+ compound of the formula (11)) (c142)n''', 1 with a compound of the formula (], c) R-OH in the presence of an alcohol.

Compounds of formulas (1) and (3) and methods for their preparation are described, for example, in US Pat. No. 3,210,313.

Examples of starting materials for formula (1a) are the following anhydrides.

maleic anhydride, dimethylmaleic anhydride, dichloromaleic anhydride, succinic anhydride, dimethylcohelic anhydride, citraconic anhydride, Kurtaric anhydride, itaconic anhydride, tartaconic anhydride, phthalic anhydride, tetracrophthalic anhydride, tetrahydrophthalic anhydride, Hexahydrophthalic anhydride.

Examples of starting materials of formula (1b) are .alpha.-pyrrolone, .alpha.-piperione or, preferably, .epsilon.-caprolactam.

Examples of the alcohol of formula (1c) are methanol, ethanol, n-butanol, 5ec-butanol, tert-phthanol, amyl alcohol, hexanol, 2-ethylhexanol, octyl alcohol, decyl alcohol, dodecyl alcohol, cyclohexanol, pencil alcohol, etc. These can be used alone or as a mixture.

The substituent Y in formula (2) advantageously has 8 to 12 carbon atoms, preferably α-methylbenzyl, α
, α-dimethylbenzyl α-tolylethyl or α-
It is xylylethyl. α-Methyl pencil is particularly preferred.

(Alkylene-O). The chains are preferably of the ethylene glycol, propylene/ethylene glycol or ethylene/propylene glycol type, with particular preference being given to the first-mentioned type.

n is preferably 4 to 40.

The acid group X is derived from a small cyclocarphonic acid, such as maleic acid, succinic acid or sulfosuccinic acid, and is attached to the alkyleneoxy portion of the molecule through an ester bridge. However, it is particularly preferred if X is derived from an inorganic polybasic acid such as sulfuric acid or or-1-phosphoric acid.

The acid group X can be present in free acid form or in salt form. As salts, alkali metal salts, ammonium salts or amine salts come into consideration. For example, lithium salt, sodium salt,
These are potassium salt, ammonium salt, trimethylamine salt, diethylamine salt, ethanolamine salt, jetanolamine salt, and triethanolamine salt. Alkali metal salts or triethanolamine salts are preferred. Monoethanolamine salt or jetanolamine salt is further 1
It can be etherified with 4 to 4 oxyethylene units.

A preferred acidic ester of component (B) has the following formula.

(Yl)m In the formula, YI is α-methylhensyl, α,α-cymedylpencyl or α-tolylethyl, xI is an acid group of sulfuric acid or preferably an acid group of orthophosphoric acid, m is 1 to 3, and n2 is 4 to 40. be.

These acidic esters are preferably sodium salts,
It takes the form of a potassium salt, an ammonium salt, a diethylamine salt, a triethylamine salt, a jetanolamine salt or a 1-reethanolamine salt.

The acidic ester of formula (2) or formula (4) suitable as component (B) is prepared by adding alkylene oxide (ethylene oxide or propylene oxide) to a substituted phenol compound as exemplified above, and forming the adduct. Polybasic oxygenated acids or functional derivatives of such acids such as acid anhydrides, acid halides, acid esters or acid amides are used to convert the acid esters and optionally the resulting acidic Nisder is further processed as described above. It is produced by converting it into a salt. Specific examples of functional derivatives include phosphorus pentoxide,
Examples include phosphorus oxytrichloride, chlorosulfonic acid, and sulfamino acid. Both the addition of the alkylene oxide and the esterification of the adduct can be carried out by known methods.

Component (B) includes phenols containing at least one α-tolylethyl group, α-methylbenzyl group or α,α-dimethylhensyl group, such as α-tolylethylphenol, α-methylpencylphenol, bis-
(α-methylpencyl)phenol or tris-(α
Very suitable are acidic esters or salts thereof, which are polyadducts prepared by adding 4 to 40 moles of ethylene oxide to 1 mole of phenol (methylpencil). These acidic esters can be used alone or in mixtures.

Esters of particular interest are phosphoric acid esters or sulfuric acid esters of adducts obtained by adding 8 to 30 moles of ethylene oxide to 1 mole of the compound obtained by adding 1 to 3 moles of styrene to 1 mole of phenol. be. In this case, the phosphoric acid ester is preferably present as a mixture of monoester and diester salts.

The preparation of the styrene additives is carried out by known methods, preferably in the presence of a catalyst such as sulfuric acid, p-)luenesulfonic acid or zinc chloride.

Suitable styrenes are unsubstituted styrene, alpha-methylstyrene or vinyltoluene (4-methylstyrene). Examples of phenols are unsubstituted phenols, fresoles, xylenols.

Particularly preferred are the phosphoric acid esters (monoesters and diesters) or sulfuric acid acid Nisdel of the alkoxylation products of the formula:

In the formula, m is 1 to 3 and n3 is 12 to 30.

Examples of alkoxylation products of formulas (4) and (5) include: 18 of ethylene oxide, an adduct of 2 moles of styrene to 1 mole of phenol;
Alkoxylation product with 18 units of ethylene oxide, adduct of 1 mole of phenol with 3 moles of styrene, adduct with 1 mole of phenol with 2 moles of 4-methylstyrene an alkoxylated product with 27 units of ethylene oxide, an adduct of 3 moles of 4-methylstyrene added to 1 mole of phenol, 1 of ethylene oxide;
Alkoxylation product with 7 units, 1 of phenol
an alkoxylation product with 18 units of ethylene oxide of a mixture of an adduct of 2 moles of styrene to 1 mole of phenol and 3 moles of styrene to 1 mole of phenol; Alkoxylation product with 13 units of ethylene oxide of a mixture of 2 moles of adduct and 3 moles of styrene to 1 mole of phenol.

The nonionic surfactants used as component (C) are advantageously alkylene oxide adducts, such as 2 to 100 moles of alkylene oxide, such as ethylene oxide and/or propylene oxide, added to 1 mole of one of the following compounds: are: aliphatic monoalcohols with at least 4 carbon atoms, preferably trivalent to hexavalent aliphatic alcohols with 3 to 6 carbon atoms, unsubstituted or C4CI 2-alkyl, phenyl, Phenols substituted by α-1-lylethyl, benzyl, α-methylpencil or α,α-dimethylpencil, fatty acids having 8 to 22 carbon atoms.

Examples of nonionic surfactants include the following:

(a) Adducts of preferably 2 to 80 mol of alkylene oxide, especially ethylene oxide, to: unsaturated or saturated higher monoalcohols having 8 to 22 carbon atoms; I fatty acids having 8 to 22
fatty amines or fatty acid amides with 1 carbon atoms, pencil alcohols, phenylphenols, pencil phenols, β-phenethylphenols, α-methylpencylphenols, α,α-dimethylpencylphenols, α-tolylethyl Phenols or alkyl moieties or at least 4
Alkylphenols having 5 carbon atoms.

In this case, it is possible to replace individual ethylene oxide units with substituted epoxides such as styrene oxide and/or propylene oxide.

(b) Alkylene oxides, especially ethylene oxide and/or propylene oxide condensation products (floc polymers).

(c) Adducts of ethylene oxide/propylene oxide to fatty amines or cyamines, especially ethylene cyamine.

(d) a fatty acid having from 8 to 22 carbon atoms and at least one
a primary or secondary amine containing two hy-1-roxy-lower alkyl groups or a lower alkoxy-lower alkyl group, or an alkylene oxide adduct of such a reaction product containing a hydroxyalkyl group. In this case, the reaction is carried out at a molar ratio of hydroxyalkylamine to fatty acid of l=1 or more than 1, for example 1:1 to 2.
・Implement it so that it is l.

(e) Sorbitan nisdel, preferably with C6C24-fatty acid ester groups, or polyethoxylated sorbitan esters, such as polyoxyethylene-sorbitan monolaurate or monoolein, in each case with 4 to 20 ethylene oxide groups; Acid ester or monostearate ester, or poly4xyethylene-sorbitan 1-lioleic acid ester having 4 to 20 units of ethylene oxide.

(f) Fatty alcohol polyglycol mixed needles, especially aliphatic monoalcohols having 8 to 22 carbon atoms, preferably alkanols having 8 to 16 carbon atoms, with 3 to 30 mol ethylene oxide and 3 to 30 mol Addition of liquefied propylene.

Among these, an alkoxylated product of the formula (5) derived from a styrene additive is particularly preferred as a nonionic surfactant.

Other particularly preferred nonionic surfactants have the formula %formula% or expression It is expressed as follows.

In the above formula, R' is an alkyl or alkenyl group each having 8 to 24 carbon atoms, or % (2) is an aliphatic group having 8 to 30 carbon atoms, 2 is 1 to 25, and Y, m, n and alkylene have the above meanings.

The compound of formula (6) has the formula R'-0-(alkylene-Q)
reacting the adduct of n, H with fatty acid T-COOH,
Alternatively, it can be produced by reacting an alcohol or phenol compound of R"-○H with a fatty acid ester of the formula T-Co-(alkylene-Q)n-T().

(■Ha□ adduct, formaldehy 1~ or formaldehy 1
~donor such as paraformaldehyde, and the formula r
-co-o-(cH2ci-r2o), ■-■,
It is a reaction product produced from wildflower ester. Some of these compounds are described in Japanese Patent Publication No. 5818486. Formula (7) not listed there
Compounds corresponding to can be produced according to the method described in the publication. In this case, the desired product of formula (7) can be obtained according to the reaction conditions described in the publication.

Compounds of the formula below are also highly suitable as component (C).

where R1 is an alkyl or alkenyl group each having 8 to 22 carbon atoms; Z and 72 are either phenyl or hydrogen; S is 4 to 80;

The compound of formula (8) has the formula R゛-0-(Q(2C horse 0),
-H.

It is produced by adding styrene oxide to polyethylene glycol ether.

The novel dyeing aid composition according to the present invention comprises the component (A)
, (B), (C) and optionally further water and stirred together, a homogeneous and transparent mixture with excellent transport and storage stability can be produced. The dyeing aids according to the invention are very stable even at high temperatures of up to 130° C. when used in dye baths.

The composition can improve the dispersion rate of the dye when dyeing polyester fiber materials, especially linear polyester fiber materials.

The invention therefore also relates to a process for dyeing old boriesul fibers using disperse dyes, and the process according to the invention is characterized in that the material is dyed in the presence of the auxiliary mixture according to the invention.

The amount of the auxiliary mixture according to the invention added to the dyebath is Dyebath 19
．． 0.3 to 6 g, preferably 0.5 to 4 g.

Examples of polyester m-string materials, especially textile fiber materials, which can be dyed in the presence of the novel auxiliary mixtures according to the invention are cellulose ester fibers, such as cellulose acetate fibers and cellulose triacetate fibers, and especially linear polyester fibers. Here, linear polyester/cotton is obtained, for example, by condensation of terephthalic acid and ethylene glycol, or by condensation of isophthalic acid or terephthalic acid and 1,4-his-(h-l-'roxymethyl)-cyclohexane. Synthesis! ltm and copolymers obtained from terephthalic acid, isophthalic acid and ethylene glycol. Linear polyesters which have hitherto been used almost exclusively in the textile industry are those consisting of terephthalic acid and ethylene glycol.

The fibrous material may also be a blend of the same or different types of fibers. For example, it may be a blended fabric of polyacrylic polyester/polyester, polyamide/polyester, polyester/cotton, polyester/viscose, polynisdel/wool, and the like.

The i-string material to be dyed can belong to various processing stages. Suitable forms include, for example: Loose fibres, fabrics such as knitted or woven fabrics, yarns in the form of packages or muffs.

Yarn packaging density is 200-600g/cm3
In particular, it can be between 400 and 450 g/cm3.

The disperse dyes used are dyes that are poorly soluble in water and exist mostly in the form of fine dispersions in the dyebath, and belong to a very wide variety of dyes, such as acrylic dyes, Aso dyes, anl-laquinone dyes, coumarin dyes,
Examples include methine dyes, perinone dyes, quinophthalone dyes, naphthoquinone imine dyes, styryl dyes, and 21-lo dyes.

It is also possible to use mixtures of disperse dyes t-'1 according to the method of the invention. The mixtures are used in particular to obtain mixed level dyeings such as two-tone and three-tone dyeings. Tricolor dyeing is especially the basic colors of yellow (or orange), red,
A combination of blue.

The amount of dye added to the dye bath depends on the desired dye density;
- Generally 0.01 to 0.01 based on the material to be dyed],
0% by weight, and 0.05 to 5% by weight gives good results.

The auxiliary mixture according to the invention can be used in admixture with known carrier carriers. Known carriers include:
For example, C- or trichlorobenzene, methylbenzene, ethylbenzene, 0-phenylphenol, pencilphenol, diphenyl ether, chlorobiphenyl, methylbiphenyl, cyclohegisanone, acetophenone, alkylphenoxyethanol, mono-, C- or trichlorophenoxyethanol or -propanol, pentachloro Examples include those based on phenoxyethanol or, in particular, those based on biphenyl, methyl biphenyl ether or dibenzyl ether. The carrier is preferably used in an amount of 0.5 to 2 g/l or 10 to 60% by weight, based on the auxiliary mixture.

Depending on the type of fiber material to be dyed, the dyebath may contain, in addition to the dyestuff and the auxiliary mixture according to the invention, also oligomeric inhibitors, antifoaming agents (for example silicone oils or ethylene-bis-fatty acid amides), anti-wrinkle agents and, in particular, dispersants. It can also contain things such as.

Dispersants achieve particularly good dispersion of disperse dyes. As the dispersant, any known dispersant that is commonly used when dyeing with disperse dyes is suitable.

Suitable dispersants are listed below.

Polyhydric aliphatic alcohols having 2 to 6 carbon atoms, such as ethylene glycol, chrycerin or pentaerythritol, or having 2 to 9 carbon atoms and at least two amino groups or one amino group and one 15 to 1 of ethylene oxide or preferably propylene oxide to the amine containing the 1-hydroxyl group.
00 moles of adducts, preferably sulfated or phosphorylated; alkyl sulfonates with 10 to 20 carbon atoms in the alkyl chain; linear chains with 8 to 20 carbon atoms in the alkyl chain. Alkylbenzenesulfonates having a straight or branched alkyl chain, such as nonylbenzenesulfonate, dodecylbenzenesulfonate, 1,3,5,7-teri-methyloctylbenzenesulfonate or octadecylbenzenesulfonate. N-1~: Alkylnaphthalene sulfonates or sulfosuccinic acid esters such as dioctylsulfosuccinate or sodium di-2-ethylhexylsulfosuccinate.

The following have also been found to be particularly useful as anionic dispersants:

Likunin sulfonates, polyphosphates, aromatic sulfonic acids, formaldehyde 1 made from formaldehyde and monofunctional or difunctional phenols, condensation products such as cresol, condensation products from β-naphtholsulfonic acid and formaldehyde condensation products from benzenesulfonic acid, formaldehyde and naphthalenesulfonic acid, condensation products from naphthalenesulfonic acid and formaldehyde, condensation products from naphthalenesulfonic acid, dihydroxydiphenylsulfone and formaldehyde.

Preferred is the disodium salt of cy(6-sulfonaphth-2yl)-methane or the disodium salt of cy(6-sulfonaphth-2-yl)-methane.

Mixtures of deionizing dispersants may also be used. These anionic dispersants are usually present in the form of their alkali metal, ammonium or amine salts. These dispersants are preferably used in amounts of 0.5 to 8 g per bath.

The dyebath may also contain a water-soluble alkaline earth metal salt, aluminum salt or organic ammonium salt of a monobasic or polybasic aliphatic carboxylic acid or a monobasic or polybasic inorganic acid. By adding these salts, the stability of the dispersion in the dyebath can be significantly improved. Depending on the type of dye used, a significant increase in stability can be achieved, especially when dyeing highly filled polyester packages. Therefore, dye deposition can be prevented or significantly suppressed. These additionally used salts are water-soluble salts, such as monobasic or polybasic inorganic acids or monobasic or polybasic aliphatic carboxylic acids, such as hydrochloric acid, Magnesium salts, calcium salts, baliwaum salts, strontium salts, aluminum salts or organic ammonium salts of hydrobromic acid, hydrofluoric acid, nitric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, thiocyanate, etc. are considered. Particular examples include calcium nitrate, macnesium nitrate, aluminum nitrate, calcium chloride, macnesium chloride, macnesium thiocyanate, calcium thiocyanate, or organic ammonium chlorides, bromides or iodides, such as methonium salts (alkanbistrimethylammonium salts). It is. Examples of suitable methonium salts are pentamethonium iodide, decamethonium bromide or especially hexamethonium chloride.

These salts are preferably present in amounts of Ool to 3 g per dyebath or 0.2 to 5% by weight based on the textile material.
used in amounts of

The dyebath furthermore contains customary additives, preferably electrolytes and/or
or may contain an acid. Examples of electrolytes are sodium sulfate,
Examples include salts such as ammonium sulfate, monohelium phosphate, ammonium phosphate, sodium polyphosphate, ammonium polyphosphate, ammonium acetate, and sodium acetate. Examples of acids are mineral acids such as sulfuric acid, phosphoric acid, or organic acids, preferably lower aliphatic carboxylic acids such as formic acid, acetic acid, citric acid, citric acid, and soybean acid.

These acids are used in particular for the PL+ adjustment of the dyebaths used. The pH value of the bath is usually between 4 and 6.5. Preferably it is 4.5 to 6.

Dyeing is preferably carried out by the exhaust method from an aqueous bath. Therefore, the bath ratio can be selected from a wide range. For example, 3:1 to 100:1. Preferably, it may range from 7:l to 5o:1. The dyeing temperature is at least 7
0°C7 and, in principle, do not exceed 140°C. Preferably it is in the range of 80 to 135°C.

Linear polyester fibers and cellulose triacetate fibers are preferably dyed by the so-called high-temperature process in closed, preferably pressure-resistant equipment at temperatures above 100°C, preferably at temperatures of 110 to 135°C under pressure. be done. Suitable closed dyeing machines are circulating machines such as package or beam dyers, Winspec, nozzle or drum dyers, shed or muff dyers, paddle dyers, jiggers, etc.

Cellulose acetate fibers are preferably dyed at a temperature of 80-85°C.

Dyeing may be carried out in the order in which the object to be dyed is first briefly treated with the auxiliary mixture and then dyeing is carried out.
It is preferable to treat the object to be dyed with the auxiliary mixture and the dye simultaneously.

Preferably, staining is carried out as follows. That is, the object to be dyed is placed in a bath containing a dye and an auxiliary mixture, and optionally additives, and whose pH is adjusted to 4.5 to 6, and preliminarily heated at a temperature of 40 to 80°C. 5
Stain for 10 minutes. The bath temperature is then increased to 110-135°C, preferably 125-130°C, for 15-30 minutes. The dyebath is then held at this temperature for 15 to 30 minutes, preferably 15 to 20 minutes.

The dyeing is completed by allowing the dyebath to cool to 60 to 80° C., and the dyed product is washed with water and optionally reduced and washed in a conventional manner in an alkaline medium under reducing conditions. After this, the dyed material is re-strained and washed and dried. This results in a level and clear dyed product. Furthermore, synthetic fiber materials dyed in this way, especially linear polyester fibers, exhibit good light and rub fastness properties. During dyeing, the dyebath is stable and does not produce sediment inside the dyeing machine.

Compared to known processes using disperse dyes that do not migrate or migrate only slowly, the process according to the invention has the advantage that the heating step is shortened and that the dye can be added to the bath at the desired temperature. There is a characteristic. especially,
The migration of disperse dyes can be improved by using the auxiliary mixtures according to the invention. By improving the transferability of the dye, uneven dyeing can be leveled in the dye absorption stage, and the level of level dyeing can be further improved by the transfer of the dye in the subsequent final temperature holding stage. In summary, the following advantages are obtained when dyeing is carried out using the auxiliary mixture according to the invention:

(b) The dyebath can be heated unsupervised to the dyeing temperature without paying special attention to the maximum permissible or critical speed of dyeing.

(b) Improved microclosing properties of disperse dyes allow for color correction under conventional high temperature dyeing conditions.

(c) Easy, efficient and reliable staining is guaranteed.

(d) Since the level dyeing property has been improved, it is possible to easily correct color differences in dyed products.

(Po)? Even in the case of mixed dyeings, including li-color dyeing and trichrome dyeing, level dyeing is quickly achieved and does not cause staining, and good color fastness is achieved even under harsh environmental conditions.
For example, excellent light fastness, abrasion fastness, and sublimation fastness are guaranteed.

(b) In most cases, dyeing can be carried out without the addition of conventional carriers, dispersants and/or leveling agents.

(g) It is possible to achieve level dyeing in light to medium colors, and it is also possible to dye in deep colors using particularly sublimation-fast dyes.

Hereinafter, the present invention will be further explained by examples. Parts in the examples are parts by weight and percentages are percent by weight.

80 parts of a polyester knitted fabric (225 g/g) was placed in a bath heated to 70°C. This bath contained the following ingredients in 1000 parts of water.

Ammonium sulfate (anhydrous) 2g/Dispersion mixture of dyes below 9°: Dye of the following formula 0.24g/text 0-28g dye of the formula below/Bunbe H (Ke'13) 0.19g dye of the formula below/composition below Auxiliary composition 1g/cross 2-ethylhexyl-6-phthalimide hexanoate
60%.

Toiethanolamine salt of a mixture of phosphoric acid monoester and diester of an alkoxylation product with 18 units of ethylene oxide of an adduct of 3 moles of styrene to 1 mole of phenol 20%.

20% alkoxylation product of 18 moles of ethylene oxide with 1 mole of adduct of 3 moles of styrene to 1 mole of phenol.

The IlH value of the bath was adjusted to pl (5) with formic acid.

This dye bath was heated to 130°C for 20 minutes while being continuously circulated, and dyeing was carried out at this temperature for 15 minutes. After this, the dyebath was cooled, drained, and the dyed material was rinsed and dried.

A dyed product with high dyeing yield and level dyeing without fading was obtained. This dyed product had excellent fastness during use. Normal reductive cleaning treatment was not necessary.

The 2-ethylhexyl-6-phthalimide hexanoate used was produced by the following method.

148 g of phthalic anhydride (-113 g of caprolactam)
, 132 g of 2-hetylhexanol, 1.9 g of P-toluenesulfonic acid and 70 g of 1,3-xylene are added and heated to 180°C. The raw water is removed by co-clearing distillation. The reaction was completed in 12 hours, during which time 18 m
1 of water is removed. After this, the solvent is evaporated in vacuo. 370 g of a compound of the following formula are obtained in the form of a brown oil.

The acid value is 6.

100 parts of a knitted fabric made of processed polyester fibers were placed in a nearly full bath heated to 60 DEG C. in a Schott dyeing machine. This bath contains 1000 parts of water, 2 parts of ammonium sulfate, a finely dispersed mixture of the following dyes and the auxiliary composition Ig as described in Example 1.
The pH of the bath was adjusted to 5 with formic acid.

Disperse Yellow 23 C, 1,260700
, 5 parts, 0.14 parts of a dye of the following formula, 0.23 parts of a dye of the following formula.

It contained 1.5 parts of formic acid, and the rol+ of the bath was adjusted to 5.

The temperature of the dyebath was increased to 130° C. over 30 minutes, and dyeing was carried out at this temperature for 30 minutes. After this, to correct the color, the pH value of the bath was adjusted to p115 using formic acid.

The temperature of the dyebath was increased to 130° C. in 30 minutes and dyeing was carried out at this temperature for 60 minutes. After this the dyebath was cooled to 90° C., drained, the dyed material was rinsed and dried without reduction cleaning. A brown level dyeing with good fastness properties was obtained.

100 parts of a knitted fabric made of processed polyester fibers were placed in a nearly full bath heated to 60°C in a Schott dyeing machine. This bath contained 1000 parts of water, 2 parts of ammonium sulfate, and finely dispersed dyes (Disperse Yellow 42', Ci,
10:138) and 0.1 part of the dyestuff of the auxiliary composition described in Example 1 were introduced into the dyebath and the knitted fabric was then dyed for a further 30 minutes at 130°C. After this the dyebath was cooled, the dyed material was rinsed and finished according to conventional methods. A bright green level dyeing with good fastness properties was obtained. As a result of the addition of the auxiliary composition described above, there was no need to cool the dyebath before adding the color correcting dye. This method therefore saves time and energy.

Claims (1)

[Claims] 1. A dyeing aid mixture containing at least the following three components: (A) Formula (1) ▲ Numerical formula, chemical formula, table, etc. ▼ (In the formula, W is at least two carbon atoms R is an aliphatic, araliphatic or cycloaliphatic group having not more than 24 carbon atoms, n is from 2 to 25); B) Formula (2) ▲ Numerical formulas, chemical formulas, tables, etc. ▼ (In the formula, V is hydrogen or methyl, X is an acid group of an oxygen-containing inorganic acid or a residue of an organic acid, and Y is α-methylaral. Kyl group, alkylene is ethylene or propylene group, m is 1 to 3, m_1 is 1 or 2, n_2 is 4 to 5
(C) A nonionic surfactant. 2. W in formula (1) is unsubstituted phenylene, halogen, C_1-C_4-alkyl or C_1-
2. Auxiliary mixture according to claim 1, which is phenylene substituted by C_4-alkoxy. 3. The auxiliary mixture according to claim 1, wherein R in formula (1) is alkyl having 1 to 12 carbon atoms. 4. The auxiliary mixture according to claim 1, wherein n in formula (1) is 5. 5. Dicarboximide ester has the following structural formula (3) ▲ Numerical formula, chemical formula, table, etc. ▼ (In the formula, W_1 is alkylene or alkenylene having 2 to 4 carbon atoms, cyclohexylene, or unsubstituted 2. Auxiliary mixture according to claim 1, having the structure: phenylene substituted by halogen, methyl or methoxy; R_1 means alkyl having 1 to 12 carbon atoms, cyclohexyl or benzyl. 6. The auxiliary mixture according to claim 1, wherein component (A) is C_3-C_8-alkylphthalimidohexanoate. 7. The auxiliary mixture according to claim 1, wherein component (A) is 2-ethylhexyl phthalimidohexanoate. 8. The auxiliary mixture according to claim 1, wherein Y in formula (2) is α-tolylethyl, α-xylylethyl, α,α-dimethylbenzyl or α-methylbenzyl. 9. The mixture according to claim 1, wherein n_1 in formula (2) is a number from 4 to 40. 10. The auxiliary mixture according to claim 1, wherein the acid group X in formula (2) is an acid group of sulfuric acid or orthophosphoric acid. 11. Component (B) has the following structural formula (4) ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ (In the formula, Y_1 is α-methylbenzyl, α,α-dimethylbenzyl or α-tolylethyl, The auxiliary mixture according to claim 1, which is a compound of the acid group of an acid, m is 1 to 3, and n_2 is 4 to 40. 12. Component (B) is 8 to 30 moles of ethylene oxide to 1 mole of a compound produced by adding 1 to 3 moles of styrene, α-methylstyrene or vinyltoluene to 1 mole of phenol, cresol or xylenol. 2. The auxiliary mixture according to claim 1, which is a phosphoric or sulfuric acid ester of an alkoxylated product or a salt thereof. 13. Component (B) is a phosphoric acid acid or sulfuric acid acid of an alkoxylation product of the formula ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ (in the formula, m is 1 to 3, and n_3 is 12 to 30) The auxiliary mixture according to claim 1, which is an ester or a salt thereof. 14. Component (C) is 1 mol of an aliphatic monoalcohol having at least 4 carbon atoms, or 1 mol of a trivalent to hexavalent aliphatic alcohol having 3 to 6 carbon atoms, substituted 1 mole of phenol free or substituted by C_4-C_1_2-alkyl, phenyl, α-tolylethyl, benzyl, α-methylbenzyl or α,α-dimethylbenzyl, or 1 mole of a fatty acid having 8 to 22 carbon atoms The auxiliary mixture according to claim 1, which is an alkylene oxide adduct in which 2 to 100 moles of alkylene oxide are added to each mole. 15. The auxiliary agent according to claim 1, wherein component (C) is an alkoxylated adduct having the formula ▲a mathematical formula, a chemical formula, a table, etc.▼ (in the formula, m is 1 to 3 and n_3 is 12 to 30) agent mixture. 16. Component (C) is the formula (6) ▲ Numerical formula, chemical formula, table, etc. ▼ [In the formula, R' means an alkyl group or alkenyl group each having 8 to 24 carbon atoms, or Formula 6 (a) ▲ Numerical formulas, chemical formulas, tables, etc. The auxiliary mixture according to claim 1, which is a compound of an aliphatic group having a carbon atom, alkylene is an ethylene or propylene group, m is 1 to 3 and n_1 is 4 to 50. 17. Component (C) is the formula (7) ▲ Numerical formula, chemical formula, table, etc. ▼ (In the formula, T is an aliphatic group having 8 to 30 carbon atoms, z is 1 to 25, Y is α - methylaralkyl group, alkylene means ethylene or propylene group, m is 1 to 3 and n_1 is 4 to 50). 18. Component (C) is the formula (8) ▲ Numerical formula, chemical formula, table, etc. ▼ (In the formula, R" is an alkyl group or alkenyl group each having 8 to 22 carbon atoms, The auxiliary mixture according to claim 1, wherein one is phenyl and the other is hydrogen, and s is from 4 to 80. %, 15 to 40% by weight of component (B), and 15 to 40% by weight of component (C). 20. Dyeing a fiber material containing polyester fibers with a disperse dye. A method characterized in that the fiber material is dyed in the presence of an auxiliary mixture according to claim 1.