CS208673B2

CS208673B2 - Method of maksng the pigment preparations with the contents of 3 to 30% weight pigments for dying the linear polyesters in the substance

Info

Publication number: CS208673B2
Application number: CS795284A
Authority: CS
Inventors: Andreas Laely; Guenther Zwahlen; Lothar Buxbaum
Original assignee: Ciba Geigy Ag
Priority date: 1979-06-21
Filing date: 1979-07-30
Publication date: 1981-09-15

Description

208674 (11) \ t <B2)

SOCIALISTIC AND DESCRIPTION OF THE INVENTION

REPUBLIC

PATENT

(22) Registered 30 07 79 (21) (PV 5284-79) (32) (31) (33) Priority from 21 06 79 (5803/79) Switzerland (51) IntCl.3 D 01 P 1 / 04C 09 B 67/08 (40) Published 3 '12 80

OFFICE OFFICE

AOBIEVY (45) published 15 03 84 (72) Author of the invention (73) Patent holder LAELY ANDHBAS dr., ALLSCHWIL, ZWAHLEN gONTHBR, SOSNÁCH (SWITZERLAND) aBUXBAUM LOTHAR dr., LINDENFELS / ODENWALD (USB) CIBA-GEIGX AG, BASILE ( SWITZERLAND (54) Method of producing pigment preparations containing 3 to 30% by weight of pigments for coloring linear polyesters 1

It is known that linear polyesters are dyed in the mass using a masterbatch. In this process, a pigment-mixed thermoplastic resin in the form of granulate, powder or pulp is added to the spinning polyester material. In the process of British Patent Specification No. 1,044,378, a pigment concentrate is produced by plasticizing a mixture of a pigment and a low melting polyester and then incorporating a higher melting point into the color of the polyester 8.

In most cases, the pigment concentrate obtained by kneading by kneading does not have the necessary dispersion and fineness of the pigment for coloring in the mass, which is particularly disadvantageous when coloring with organic pigments.

This is manifested, for example, by an unacceptable increase in pressure in the tissue spinning apparatus, in increased fiber breakage rates, in poor drawability, by adverse effects on the textile characteristics, and not, in the end, by the poor coloring effect. In the process described in U.S. Pat. No. 4,012,358, it is proposed to avoid such difficulties by first preparing a precondensate from 50 to 75 parts of pigment and 50 to 25 parts of polyethylene which is melted with one to four times the amount of fiberizable polyester and processed the granulate.

The lack of this method is based on the fact that the polyethylene and the polyester do not tolerate a significant tendency to form two phases, thereby obtaining a non-homogeneous mixture which in turn can adversely affect the spinning and drawing behavior and the properties of the produced polyester fibers. Also, the normal, non-conditioned fresh air in the weaving hall 51, as well as the air purge through the inlet ducts 2, 1, can be fed to the air to serve inside the machine. 208673 2

We have now found a process for the production of pigment preparations for the dyeing of linear polyesters in a mass which does not have the drawbacks of the two prior art processes and leads to a product and extraordinary fine dispersion of the pigment in the spunbonded resin.

The process according to the invention is characterized in that a pre-concentrate of 20 to 80 parts by weight is produced and 80 to 20 parts by weight of polyester having a melting point of 60 to 160 ° C is kneaded with a salt solvent or a phase exchange process which is melt spun by a linear polymer and processed the granulate. Preferably, 40 to 60 parts of pigment and 60 to 40 parts of polyester are used to prepare the preconcentrate. The pigment and polyester pre-concentrate is preferably melted and granulated in a quantity which is linearized with a linear polyester so that the granulate contains 3 to 30% by weight, preferably 5 to 25% by weight, of pigment.

Possible pigments are both inorganic and organic pigments which are stable in polyester, with organic pigments being preferred. Asorganic pigments are exemplified by: metal oxides and sulfides, ultramarine, white pigments such as titanium dioxide and other inorganic pigments. Preferred organic pigments include, in addition to carbon black, all known pigments suitable for dyeing polyester polyesters, such as pigments of the azo pigments, azomethine pigments, anthraquinone pigments, chinophthalone, phthaloeyanine, perinone, pentylentetracarboxylic acid diimide pigments, acid dianhydride pigments pylentetracarboxylic acid, dioxazine, thioindigo, iminoisoindolinone or quinacridone pigments.

Also suitable are metal complexes, such as azo-dyes, azomethine or methine dyes with the character of pigments.

Linear thermoplastic polyesters based on aromatic or aliphatic dicarboxylic acids or mixtures of aromatic and aliphatic dicarboxylic acids with aliphatic diols can be used as polyesters.

Aromatic dicarboxylic acids are, for example, terephthalic acid or isophthalic acid. Suitable aliphatic dicarboxylic acids are linear or branched dlcarbosyl acids having up to 20 carbon atoms, preferably 4 to 12 carbon atoms.

Examples are azelaic acid, sebacic acid and adipic acid. Examples of diol are ethylene glycol, 1,4-butanediol, 1,4-di (hydroxymethyl) cyclohexane or neopentyl glycol, which are condensed with dicarboxylic acids to give a polycondensate whose molecular weight is preferably 18,000 to 30,000 and has a melting point of 60. up to 160 ° C, preferably 100 to 160 ° C.

Especially preferred for the process according to the invention are polyesters which comprise: a) 25 to 30 mol% of terephthalic acid residues, 20 to 25 mol% of azelaic acid residues or equal by weight of aliphatic dicarboxylic acid residues of 4 to 12 carbon atoms and b) 50 % mole residues of butanediol and diethylene glycol or triethylene glycol in a ratio of 5: 1 to 5: 1. In this polyester, about 7 mole% of terephthalic acid residues can be replaced by isophthalic acid residues. Also, diethylene glycol may contain up to 20 wt. ethylene glycol. 3 208673

The polyesters used according to the invention are preferably at least partially soluble in diacetone alcohol and / or dimethylformamide, optionally in a mixture of acetone and dimethylformamide, at a temperature of 80 to 90 °. The pigment and polyester precondensate is preferably produced by kneading in a solvent and salt, thereby achieving the best possible fineness and dispersion of the pigment in the polyester. The treatment is preferably carried out at elevated temperature, for example at 80 to 95 ° C, in the presence of an inorganic salt, in particular sodium chloride, and also potassium chloride, sodium sulfate or barium chloride.

The salts can then be washed away in a simple manner with water. For kneading, it is preferable to add a solvent, especially a water-soluble organic solvent such as di-acetone alcohol or dimethylformamide, in which the polyester used is at least partially soluble. After the kneading is complete, the brown matter is freed, suitably with water, with a salt, freed from the solvent and dried.

Also, good results are obtained, especially when the pigments themselves are fine, in a so-called phase exchange or flushing process, whereby the phase change or the phase change is made into a melt or a concentrated polyester solution.

Spinnable linear polyesters with which the preconcentrates obtained are melted and processed into the masterbatch are, in particular, polyesters which are obtained by polycondensation of terephthalic acid or esters thereof with glycols of the general formula

HO- (CH 2) n -OH wherein n is 2 to 10, or with 1,4-di (hydroxyethyl) cyclohexane or polycondensation glycol ethers of hydroxybenzoic acids. The term linear polyesters also includes copolyesters which are obtained by partially replacing terephthalic acid with another dicarboxylic acid or hydroxycarboxylic acid. acid and / or partial replacement of glycol with another diol.

However, polyethylene terephthalates, which are mostly identical to colored linear polyesters, are of particular importance. For the production of pigment preparations, polyethylene terephthalate is suitably mixed with a homogeneous mixture of pigment and polyester pre-concentrate by suitable methods, the mixture is melted in a single-screw or double-strand extruder or in a continuously operating brownish and transferred to a granulate.

The processing into the granulate is also free of pre-mixing in the extruder into which the finely divided pre-concentrate and polyethylene terephthalate granulate are in a desired weight ratio in a continuous manner. The desired pigment content of the granulate, preferably 5 to 25% by weight, can be achieved by adding a corresponding amount of spinable linear polyester to the pre-concentrate.

As a rule, approximately the same amount of pre-concentrate and linear polyester are melted together, and the melt is processed into a cylindrical or angular granulate. A mixture of different pigments may also be used to produce the pigment concentrate. Mixtures of different polyesters may also be used.

In addition, the two-stage process has the advantage that by the simultaneous use of pigment concentrates of different shades in the fibrous polyester, suitable homogeneous granules of special shades can be produced. Pigment pre-concentrates can also be combined with a polyester-soluble dye. 208673

The pigment preparations according to the invention make it possible to achieve a useful pigment dispersion in the polyester in the dyeing of polyester fibers in the fabric, neither the spinning process nor the drawing process being affected, nor the quality of the fibers being reduced. Despite the relatively low melting point of the polyester in the precondensate, the corresponding amount of which reaches the finished fiber, the granulated pigment preparations are not sticky and can therefore be dried at temperatures common in the fiber industry, 160 ° C, even at high temperatures.

The dyeing of the polyester with pigment preparations obtained by the process according to the invention is carried out in a manner known per se, whereby the dyed polyester, preferably in the form of a powder, cuttings or granulate, is blended with the pigment preparation, melted in an extruder and pressed into foils or fibers or is cast on plates. In this case, extrusion of the fiber formation is of particular importance, since the advantages of the dyed linear polyesters in this manner are most prominent in this method. In the following examples, parts and percentages, unless otherwise indicated, are by weight and temperatures are given in ° C. Example 1

In a heatable and cold-lit 50 liter 50-liter kneader kneader, knead 7.5 kg under the name Dynapol L 206 of the obtainable linear thermoplastic copolyester of Dynamite Nobel AQ, consisting of an aromatic dicarboxylic acid and an aliphatic diol having a molecular weight of 18,000 to 20,000 and a temperature of mp 90-115 ° C, 5.0 kgpigment red 166 by Color Index, 30.0 kg of finely ground sodium chloride and 4.5 kg of diacetone alcohol for 5 hours at a kneading temperature of 85-90 ° C. By adding water, the kneaded mass is transferred to a relatively finely granular granulate which is suspended in about 250 l of water and subjected to wet milling. The resulting suspension is filtered and washed with water to remove salts and solvent. Dry for 48 hours at 75 ° C in a vacuum oven. 5.0 kg of this fine granulate is mixed with 5.0 kg of pulverulent polyethylene terephthalate prepared either by grinding the granulate in a hammer mill with the addition of solid carbon dioxide, or by precipitation from a solution of granules, for example in gamma-butyrolactone, by addition of water, filtration drying and mixing for three hours on a roller stand, this mixture is then dried for 72 hours under vacuum at 60-70 ° C and then re-melted in a laboratory co-kneader of the List (Type PB / 4SV 46, Busa) at 175-242 ° C The wire which is cut on a cutting machine (FO1JBNE, WILCO) into a roller granulate with a diameter of 3 mm and a distance of 2-3 mm. Instead of the List co-driver, the same result can be used for the Werner & Pfleiderer Type ZDS-K28 or Leistritz twin screw extruder TypeLSM-30.34. The granulate obtained has the following composition: 20% pigment, 30% Dynapol L 206 copolyester, 50% polyethylene terephthalate; it is very well suited for dyeing polyester fibers in the fabric. 5,208,673 Example 2

In a 50-liter two-spoke jack, 9.0 kg of Byaapol L 206 (see example 1), 6.0 kg of indantrone, 24.0 kg of finely ground sodium chloride and 4.8 kg of diacetone alcohol for 4 hours at a kneaded material temperature of 85 Å 90 ° C. By adding ice, the kneaded mass is decomposed and granulated. This granulate is suspended in 250 liters of water and subjected to wet milling. It is filtered and sieved to remove salt and solvent.

It is then dried for 48 hours at 75 ° C in a vacuum oven. 5.0 kg of the thus obtained fine granulate is treated in a similar manner to that described in Example 1, with 5.0 kg of a powdered polyethylene terephthalate on a blue roller granulate (or strip granulate) which is suitable for the excellent dyeing of polyesters in the mass . Example 3

The procedure described in Example 1 is followed instead of Synapol & 20b, however, the Liuronic saturated copolyester Vesturit EL 952 of Chemische Werke HS11s is used, having a melting point of 90-130 ° C, thus obtaining a further redine suitable for dyeing polyesters in the mass. Example 4

This 50 liter two-film kneader will deliver the following kneading batch: 7.5 kg of Vesturit EL 952 (characterized in Example 3), 5.0 kg of crude copper beta-phthalene, 30.0 kg of finely ground sodium chloride, 4.5 kg of diacetone alcohol.

After a kneading time of 6 hours at 80-85 ° C, the kneaded mass is decomposed by adding water to a fine granulate which is suspended in 500 liters of water and filtered after wet milling, washing the filter cake with water to remove sodium chloride and solvent.

After drying in a vacuum oven (48 hours at 60-70 ° C), the resulting flowable, semolina 40% preparation can be worked on a blue granulate by working with the same amount of polyethylene terephthalate powder as described in Example 1. containing 20% copper beta-phthalocyanine, which is well suited for dyeing in the polyester fiber mass (the co-kneader temperature is 185 to 245 ° C). Example 5 48 parts of the commercial product Vitel VPE-38621, which is a linear saturated copolyester of Ooodyear Co., are kneaded in a laboratory tube. with a molecular weight of 20,000 to 30,000 and a melting point of 100 to 125 ° C, 32 parts of the blue pigment of Example 2, 160 parts of finely ground sodium chloride and 43 parts of diacetone alcohol for 5 hours at 90 ° C. By adding 50 parts of water, the kneaded mass is decomposed and granulated. The coarse-grained granulate is suspended in 4000 parts of water and rubbed onto a fine-grained granulate in a gear colloid mill.

After filtration, the filter cake is washed with water to remove salt and solvent and dried in a vacuum oven at 60-70 ° C. A slightly coarse powder is obtained. 150 parts of this powder are mixed with 150 parts of ground polyethylene terephthalate on a roller stand. After drying at 60 [deg.] C. and 70 [deg.] C. in a vacuum, the mixture is melted in an extruder and processed into a wire having a diameter of 3 which is then cut into a blue-roller granulate by a distance? ai 3 mm. The granulate obtained consists of 20% dye, 30% Vitel VPB-38624 copolyester and 50% polyethylene terephthalate and stabbed excellent for dyeing polyester fibers in the mass. EXAMPLE In the laboratory kneader, the following batches are kneaded: 48 parts of a terephthalic acid-based copolyester, aselalenic acid, 1,4-butanediol and diethylene glycol, m.p. 125 DEG -155 DEG C., 32 parts Carbon black Prlntex 400 from Beguesa, 128 parts finely divided sodium chloride and 38 parts. parts of dimethylformamide.

Knead for five hours at about 95 ° C and then cool to 50 ° C. The mixture is decomposed into a fine granulate by the addition of about 40 parts of ice. The granulate is added to 4000 parts of water and the suspension is filtered after stirring for several hours. The filter cake was washed to remove salt and solvent and then dried under vacuum at 60-70 ° C.

Now 200 parts of the thus obtained formulation are mixed with 200 parts of powdered polyethylene terephthalate and, after treatment as described in Example 5, a black granulate is obtained which is suitable for dyeing polyester fibers in the mass in an excellent way. Example? a) 540 parts of the granular form of the present polyethylene terephthalate are mixed with 60 parts of the granulate containing the pigment dye obtained according to the previous examples, shaken in a closed vessel or on a roller table.

The thus obtained mixture of colorless polyethylene terephthalate and the granular preparation was slurried at 100 ° C for about 48 hours and at a pressure of about 66.6 Pa and then spun into an Xnventa spinneret for spinning at a temperature of about 90 ° C. minutes and at a take-off speed of 300 m / l using a nozzle for the production of polyester filaments having 24 µm of 0.35 m 2.

The polyester filaments are then drawn on a drawing machine at a temperature of 100 ° C at a ratio of 1: 4.022. The properties of the fibers are essentially the same as those of the non-colored fiber. b) If aiaSt of unstained polyethylene terephthalate granulate and masterblue granulate was dried at 160 ° C for 24 to 48 hours, equally good results were obtained.

ExampleS

In a heatable and refrigerated 0.5 liter utility kneader, get a blend of this composition: 48 parts of Iynapol L 206 (according to Example 1), 32 parts of pigmented red 88 by Color Index, 160 parts of finely ground sodium chloride and 25.6 parts by weight acetone alcohol for 5 hours; the temperature of the kneaded mass is maintained at 78-82 ° C.

Then 55 parts of ice are added to distribute the kneaded material and to granulate. The obtained, slightly non-uniform granulate is mixed into 3,000 parts and then milled to a uniformly fine granulate 7,208,673 in a gear colloid mill. The filter cake is washed to remove salt and dehydrate; then dried in a dryer at 60-70 ° C. 100 parts of this dried composition are mixed with 100 parts of ground polyethylene terephthalate in a Turbula. Again, dry at temperatures! 60-70 ° C under vacuum and the moon is treated with an extruder at 190-230 ° C for wires of about 3µ. these wires are chopped into a roller-shaped granulate of 2 to 3 m in length on the machine bed. The abrasion-resistant granulate obtained consists of 20% pigment, 30% Dynapol L 206 copolyester and 50% polyethylene terephthalate, and is an excellent method for dyeing polyester fibers in the mass. Example 9 In a 0.5 liter commercial kneader, mix this mixture for 5 hours at 85-90 ° C: 48 parts of terephthalic acid-based copolyester, iaophthalic acid, azelaic acid, 1,4- of butanediol and diethylene glycol, with a melting point of 1 5 [mu] l and 150 [deg.] 0.32 parts by pigment color violet 23, 160 parts of finely ground sodium chloride and 43 parts of diacetonaclohol.

It is then cooled to 50 DEG C. and the kneaded mass is decomposed by adding finely divided granules to 30 parts of ice. This granulate is added to 3000 parts of water at 60-65 ° C and the resulting suspension is stirred for several hours. Filter ee and filter cake to remove salt and solvent. It is then dried under vacuum at 60 to 70 ° C. 200 parts of the preparation thus obtained are mixed with 200 parts of polyethylene terephthalate powder. This was dried in a vacuum dryer at 60-70 ° C, extruded at 180-260 ° C and processed into a 3 mm wire. This wire is cut into a violet roller granulate with a length of 2-3 mm on the cutting machine.

The granulate has the following composition: 20% dye, 30% copolyester and 50% polyethylene terephthalate. It is very suitable for dyeing polyester fibers in the mass. Example 10

The following batch will be introduced into the laboratory kneader ee: 32 Co-lour Index Yellow Pigments 129, 48 parts of the Vesturit Bb 950 commercial product, a saturated Chemische Werke Hulls copolyester with a melting point of 100 to 150 ° C, 160 parts of finely ground chlorine. sodium salt and 29 parts of diacetone alcohol.

Wipe for 4 hours at 85 to 88 ° C kneaded material, cool to 50 ° C and decompose the kneaded material by adding about 40 parts of ice to a fine granulate. This granulate is introduced into 4000 parts of water at a temperature of 70 ° C, milled to a fine uniform granulate with a toothed colloid mill and filtered.

The filter cake is washed with water to remove salt and solvent, and after drying in a vacuum oven at 0 to 70 ° C, 800 parts of the fine granulate thus obtained are mixed with 200 parts of powdered polyethylene terephthalate. This was dried under the same conditions as in Example 9 and then processed in a extruder at 18 ° to 260 ° C to wire.

This wire is cut on the cutting machine and the yellow cylindrical granulate 2-3 mm in length is suitable for excellent dyeing of polyester fibers in the mass.

The granulate has the following composition: 20% pigment, 30 $ copolyester Vesturit Bb 9 - 0 and 50 $ polyethylene terephthalate. 208673 Example 11 32 Color Slut ItO Pigmented Parts by Color Index, 48 Parts Testurit BL 951 Copolyester, a Chemische Werke HSils Commercial Product, mp 90-140 ° C, 128 parts Fine Ground Sodium Chloride, and 25.6 parts diacetone alcohol knead in the lab coater at a kneading temperature of 85 to 90 ° C for four hours.

It is then cooled to about 50 ° C, mixed with 30 parts of ice to distribute the kneaded mass to a fine granulate. This granulate is suspended in 4000 parts of water at about 60 ° C and milled to a uniformly fine granulate in a colloidal gear mill. Filter the sea filter cake with water to remove salt and solvent.

It is then dried under vacuum at 60 to 70 ° C and 150 parts of the granulate thus obtained are mixed with 150 parts of ground polyethylene terephthalate. After drying in a vacuum oven at 60-70 ° C, this mixture is melted in an extruder at a temperature of 180-260 ° C and processed at a diameter of 3 mm. 7 the wire cutter is cut into a roller granulate having a length of 2 to 3 mm. This roller granulate can, and with very good results, be used according to Example 7 to dye polyester fibers in the mass. The granulate has the following composition: 20% dye pigment, 30% Veeturit BL 95 copolymer, and 50% polyethylene terephthalate. Example 2 In a laboratory litter of 0.5 liters, heatable and refrigerated, bend for five hours at 85 ° C, 48 parts of Dynapol L 205 copolyester, a commercial product of Dynamit Nobel AG, and it is an aromatic di-carboxylic acid copolyester and an aliphatic diol having an average molecular weight of about 15,000 and a melting point of 85 to 135 ° C, 160 parts of finely ground sodium chloride, 25.6 parts of diacetone alcohol and 32 parts of quinophthalone gold orange pigment

After said kneading time, it was cooled and mixed with 30 parts of ice at a temperature of about 55 ° C to decompose the kneaded mass into a fine granulate which was suspended in 4,000 parts of water at a temperature of 60 ° C.

This suspension is processed on a colloidal gear mill. Thus, a uniformly fine granulate is obtained which, after filtration, is washed with water to remove salts and solvent. After drying under vacuum at 60 to 70 ° C, 100 parts of this granulate are mixed with 300 parts of ground polyethylene terephthalate and the mixture is dried again under vacuum at 60 to 70 ° C. In a laboratory extruder, at 180 DEG-260 DEG C., the preparation is melted into a 3 mm wire. This wire is cut into a cylindrical granulate of 2 to 3 mm in length, which is used to dye the polyester fibers in the mass as described in Example 7. The formulation has the following composition: 0% pigment, 15% Bynapol L 205 and 75% polyethylene ether phthalate . EXAMPLE 3 48 parts of an aliphatic polyester based on eebacic acid and hexanediol with an average molecular weight of 1550 and a melting point of 70-82 ° C are melted in a laboratory kneader. To this melt was added 25.5 parts of a Co-lour Index Pigment Orange 43 aqueous filter cake with a dry matter content of 25.5% and the mass was kneaded at 87 ° C until the distilled water was perfectly clear. and colorless. 40 parts of ice are added and kneaded in the presence of the total amount of water, kneaded material is excluded and added in the form of ice, followed by announcement. The kneaded mass disintegrates into a fine granulate. This granulate was dried under vacuum at 50 ° C. The parts of this granulate are mixed with 233 parts of polyethylene terephthalate and this mixture is processed in a laboratory extruder at 180 DEG to 260 DEG C. into a 3 mm wire in a laboratory extruder, after cutting in vacuum at 0 DEG C., which is chopped into a roller machine in a cutting machine. about 3 mm.

This granulate can be used with excellent results for dyeing polyester fibers in the mass as described in Example 7, with a lower pigment content of 3%.

The granulate has the following composition: 3% dye, 4.5% lifestyle polyester and 92.5% polyethyl enteraftalate. Example 1, 4

After the laboratory heatable and smoothable kneader, 48 parts of VesturituEL 952, characterized in Example 3, and 92 parts of cyclohexanone were introduced. At 88 [deg.] C., after obtaining a usable solution, 2.5.5 parts of Example 3, 3 of said aqueous orange orange 43 according to the Color Index and kneaded until the solution was clear and colorless.

The water is then poured off, the mass is cooled and the solvent is removed in vacuo at 60-70 ° C. Then the hard mass is broken and ground. The parts of the ground preparation are mixed with 10 parts of ground polyethylene terephthalate.

The mixture is dried under vacuum at 60-70 ° C and then extruded to a 3 mm diameter wire extruder at 80-260 ° S, which is cut into a 2 to 3 mm roller granulate in a cutting machine. , which is an excellent method for dyeing polyester fibers in the mass.

The granulate has the following complexity: 20% dye, 30 <Vesturite EL 952 and 50 * polyethylene terephthalate. Example, 5

Knead the following batch for 4 hours at 90 ° C in a laboratory kneader: 32 parts of pigment violet, 9 according to Color Index, 48 parts of Dynapol L 206, characterized in Example 1, 28 parts of finely ground sodium chloride and 25, 6 parts diacetone alcohol. By adding 30 parts of ice while cooling, the kneaded material is decomposed, introduced into water and milled on a cloid tooth mill to form a fine granulate. This granulate was suspended in 3,000 parts of water at about 60 ° C. it is stirred for one hour while maintaining this temperature, filtered and washed with water to remove salt and solvent, then dried in a vacuum oven at 60-70 ° C. 50 parts of dried fine granulate are mixed with 150 parts of ground polyethylene terephthalate; this mixture is vacuum vacuumed at 60-70 ° C and processed in an extruder to a temperature of 180-260 ° C on a smooth 3 mm wire which is chopped on a cutting machine with a roller size of 2-3 mm.

The granulate has the following composition: 10% dye, 15% Dynapol L 206 and 75% polyethylene terephthalate. Example 16 15 parts Color Index Pigment Red, 17 parts Beta-phthalocyanine 6di crude, 48 parts eebacic acid aliphatic polyester and ethylene glycol having a molecular weight of about 4,000 to 5,000 and a melting point of 72 to 81 ° C, 190 parts fine ground sodium chloride and 55.6 parts of diaeetone alcohol at 60 ° C for four hours in a laboratory oven.

The mass was then cooled and quenched by adding 40 parts of ice to a fine granulate. This granulate was suspended in 4,000 parts of water and counted on a fine granulate in colloidal tooth mill.

Filter ee, wash the filter cake with water to remove salt and rinse. Dry under vacuum at 50 ° C and then mix 50 parts of the granulate with 350 parts of polyethylene terephthalate in a mold 6 powder. The mass is dried and melted in an extruder at a temperature of 180-260 ° C, and then subjected to a wire cut into a granulate. The polyester fibers are dyed in the mass by means of this granulate for interesting navy blue shades.

The granulate has the following composition: 5 9 dyes, 7.5 X aliphatic polyester, 87.5 X polyethylene terephthalate. Example 17 In a heatable, cold-lit, 0.5 liter usable laboratory kneader, obtain 32 parts of Color Index Pigment B red, 48 parts of Vesturl EL 952, characterized in Example 3, 160 parts of fine ground sodium chloride and 25.6 parts of diaeetone. alcohol for four hours at 88 ° C.

It is cooled and mixed with 30 parts of ice to obtain a relatively fine granulate which is mixed into water and milled to a uniformly fine granulate in a colloidal gear mill. It is filtered off, the filter cake is washed with water to remove salt and solvent and dried in a vacuum drying oven at 60 to 70 ° C. 100 parts of dry granulate are mixed from 100 parts of ground polyethylene terephthalate. After drying under vacuum at 60 to 70 ° C, the mixture will melt 180 to 260 ° C in the extruder at a temperature of 180 to 260 ° C, which is processed in a cutting machine to form a granulate. The granulate is well suited for dyeing polyester fibers in the mass.

The granulate has the following composition: 20X dye, 30X Vesturite EL 952 and 50X polyethylene terephthalate. Example 18

The following kneaded material was processed at 85 ° C for four hours: 32 parts of Color Brown Pigment Brown, 48 parts of Dynapol L 206, characterized in the example of 1.160 parts of finely ground sodium chloride and 25.6 parts of diaeethanol.

Claims

When cooling, it is mixed with 30 parts of ice to decompose the kneaded material to form a fine granulate. This granulate is ground in an aqueous suspension on a colloidal gear mill. It is filtered and the filter cake is washed with water to remove salt and solvent and dried under vacuum at 60-70 ° C. 100 parts of this granulate are mixed with 100 parts of a copolyester of terephthalic acid, isophthalic acid, azelaic acid and ethylene glycol with a melting point of 185 to 200 ° C. The mixture was dried under vacuum at 60-70 ° C and extruder extruded at 150-230 ° C onto a wire which was cut in a chopper. The granulate obtained is well suited for dyeing polyester fibers in the mass. The granulate has the following composition: 20% of dye, 30% of copolyester Dynapol L 206 β 50 * copolyester β by melting point. If the procedure described in Examples 1 to 6, 8 to 12 and 15 to 18 is followed, the finely divided potassium chloride, calcium chloride, barium chloride or sodium sulphate is used in the sodium kneading process when kneading with salt, and are obtained equally well. suitable preparations for coloring polyesters in the mass. EXAMPLE 20 If the procedure described in Example 14 is followed, methylhexanene, benzoic acid methyl ester, methylene chloride, chloroform, 1,2-dichloroethane, tetrachlorethylene, 2-nitropropane, benzene or tetrachloromethane are used instead of cyclohexanone at phase exchange process, equally well-suited preparations for barvenipolyester fibers in the mass are obtained. DM SlDMi Ϊ VHÍ LIZ U

A process for the preparation of pigment preparations comprising from 3 to 30% by weight of pigments for the dyeing of linear polyesters in a mass, characterized in that a pre-concentrate of 20 to 80 parts of pigment and 80 to 20 parts of polyester having a melting point of 60 to 160 ° C is kneaded with salts. and the solvent or phase exchange method of the pre-concentrate is melted with a wettable linear polyester and processed into a granulate.

2. The process of claim 1 wherein the pre-concentrate is made from 40 to 60 parts of pigment and from 60 to 40 parts of polyester.

3. Process according to claim 1, characterized in that the polyester consists of the following components: 25 to 30 Si molar residues of terephthalic acid and 20 to 25 molar residues of azelaic acid or the same amount of residual aliphatic dicarbosylic acid having 4 to 12 carbon atoms; mole% of butanediol residues or ethylene glycol or triethylene glycol residues in a ratio of 15: 1 to 5: 1. Sevorogn-fia, n.