US3783650A

US3783650A - Apparatus for the processing of textiles, fibres and the like

Info

Publication number: US3783650A
Application number: US00042818A
Authority: US
Inventors: J Hertig; B Milicevic; H Weber; A Litzler; H Fuhring; J Sieber
Original assignee: Ciba AG; Boewe Boehler and Weber KG
Current assignee: BASF Schweiz AG; Boewe Boehler and Weber KG
Priority date: 1969-06-02
Filing date: 1970-06-02
Publication date: 1974-01-08
Anticipated expiration: 1991-01-08
Also published as: FR2049143B1; DE1931353A1; GB1326708A; GB1326261A; BE751264A; CH518745A; AT312547B; CS151554B2; NL7007920A; ES380239A1; DE2026283A1; FR2049143A1; CH832769A4; AT319175B

Abstract

The invention relates to a plant for the processing of textiles, fibers or the like in a liquor, in which an organic solvent immiscible with water, having a specific gravity greater than 1, and forming azeotropic mixtures with water is used.

Description

United States Patent [19] Weber et al.

[ ,Han.8,1974

APPARATUS FOR THE PROCESSING OF TEXTILES, FIBRES AND THE LIKE Inventors: Hans-Peter Weber, Basel; Alfred Litzler, ltingen; Jean Hertig, Basel; Branimir Milicevic, Riehen, all of Switzerland; Heinrich Fuhring, Augsburg; Johannes-Helmut Sieber, Aystetten, both of Germany Assignees: Ciba Limited; Bowe Bohler &

Weber KG, Maschinenfabrik, Basel, Switzerland Filed: June 2, 1970 Appl. No.: 42,818

Foreign Application Priority Data June 2, 1969 Switzerland 8327/69 June 20, I969 Germany P 19 31 353.2

US. Cl 68/18 C Int. Cl. DOM 43/08 Field of Search 68/18 C, 18 R;

244,226 12/1960 Australia 68/18C Primary ExaminerBilly J. Wilhite Assistant Examiner-Philip R. Coe Att0rneyl(arl F. Ross 5 7 l ABSTRACT The invention relates to a plant for the processing of textiles, fibers or the like in a liquor, in which an organic solvent immiscible with water, having a specific gravity greater than 1, and forming azeotropic mixtures with water is used.

8 Claims, 5 Drawing Figures mmninm 81974 QUIET 1 3 INVENTOR BY v Jul!

FAYENTED AH 8 1374 sum 2 OF 3 INVENTOR APPARATUS FOR THE PROCESSING OF TEXTILES, FIBRES AND THE LIKE FIELD OF THE INVENTION The invention relates to a plant for the processing of textiles, fibers or the like in a liquor, iii which an organic solvent immiscible with water, having a specific gravity greater than 1 and forming azeotropic mixtures with water is used.

BACKGROUND OF THE INVENTION According to the field of application involved, the liquor may consist of the solvent alone with the processing agent dissolved therein, or it may consist of an emulsion of water or of aqueous solutions (using a water-soluble processing agent) and the solvent, in

thylformamide N,N-dimethylacetamide bis- (dimethylamido )methane phosphate, tris- (dimethylamido) phosphate, N-methylpyrrolidone, 1,5-dimethylpyrollidone, N,N-dimethylmethoxyacetamide, N,N,N',N-tetramethyl urea, tetramethylene sulphone (sulpholane) and 3- methylsulpholane and dimethylsulphoxide, particularly those which, in the pure state, are capable of dissolving undiluted polyacrylonitrile.

The liquors must not contain more than 50%, and preferably not more than of the dissolving intermediary.

The substances hereinbefore described are excellently suited for the processing, for example dyeing, of cellulose, such as cotton or viscose fiber, and preferably for the processing, for example dyeing, of leather, wool, silk and particularly synthetic fibers, such as acrylic fibers made of polyacrylonitril and copolymers of acrylonitrile and other vinyl compounds, such as acrylic esters, acryloamides, vinylpyridine, vinylchloride or vinylidene chloride, copolymers of dicyanoethylene and vinylacetate and of acrylonitrile block copolymers, fibers of polyurethane, fibers of base'modified or nickel-modified or unmodified polyolefins, such as polypropylene, fibers of cellulose triand 2%-acetate, and particularly fibers of polyamides, such as nylon-6,

nylon

6,6 or nylon 12, and fibers of aromatic polyesters, such as fibres of terephthalic acid and ethylene glycol or 1,4-dimethylcyclohexane and copolymers of terephthalic acid and isophthalic acid and ethylene glycol as well as acidor base-modified polyesters.

Where emulsions (for example, perchloroethylene/- water cmulsionsof the W/O or ()/W type) are used,

emulsifying agents the presence of which is optional in.

purely organic media, have also to be used. Anionic and particularly nonionie emulsifying agents are preferably used.

Examples of anionic emulsifiers include C C fatty alcohol sulphuric acid esters; C alkylaryl sulphonates; C alkyl sulphosuccinic acid esters, products of the sulphatization of unsaturated oils and fats; C ralkylphosphon'c acid esters, and soaps of fatty acids.

The following groups of non-ionic emulsifying agents are particularly mentioned:

a. Adducts of polyalkylene oxides, such as polyoxyalkylated fatty alcohols, polyoxyalkylated polyols, polyoxyalkylated mercaptans and aliphatic amines, alkylphenols and naphthols, polyoxyalkylated alkylaryl mercaptans and alkylarylamines.

b. Fatty acid esters of ethylene-and polyethylene glycols and of propylene and butylene glycol, fatty acid esters of glycerol or polyglycerols and of penterythrite as well as fatty acid esters of sugar alcohols, such as sorbite, sorbitanes and saccharobiose or sucrose.

c. N-hydroxyalkylcarbonamides, polyoxalkylated carbonamides and sulphamides.

The dyes suitable according to the invention may belong to any optional class of dyes. They may be azo dyes which may be free from metal or may contain heavy metals, including the formazan dyes, or they may be anthraquinone, nitro, methine, azamethine, styryl, azostyryl, naphthoperinone, quinophthalone, oxazine, 5-amino-8-hydroxy-l,4-naphthaquinone of phthalocyanine dyes. Water-soluble dyes soluble in alcohols, dispersion dyes and dye salts soluble in organic solvents are particularly suitable. By dye salts or this kind are to be understood particularly those dye salts that are soluble in low alcohols, ketones and in mixtures of such so]- vents.

Water-soluble dyes are particularly the so-called acid wool dyes of the azoand anthraquinone series. Preferred azo dyes include monoor diazo dyes, particularly acid azoand anthraquinone dyes free from metal which contain only one sulphonic acid or carboxylic acid group, and azo dyes containing a heavy metal, particularly chromiumor cobalt-containing azo dyes, preferable metallized monoazo dyes free from acid groups and basic groups by which the dye is rendered water-soluble, such monoazo dyes containing 2 molecules of azo dye combined with 1 atom of metal. 1- amino-4-acylamino-anthraquinone-Z-sulphonic acids are anthraquinone dyes which should be particularly mentioned.

Preferred dyes soluble in alcohol include azo dyes and certain phthalocyanine dyes which contain no metal. Preferred phthalocyanine dyes are copper phthalocyanine sulphonic acid amides with substituted amide nitrogen.

The preferred dispersion dyes are monoazo dyes free from metal which contain no acid salt-forming groups and which may contain fiber-reactive groups.

Suitable dye salts soluble in organic solvents include particularly salts with an organic cation and an organic anion, that is to say dye salts with a colored cation and a colorless anion as well as dye salts with acolorless cation and a colored anion, and dye salts with a colored cation and a colored anion.

The colored constituent in such dye salts may be derived from any one of the aforementioned dye classes. Preferred colored cations may belong, for example, to the dyeand triphenylmethane, rhodamine, oxazine or thiazine series, or they may be azo dyes containing quaternary ammonium groups and particularly cycloammonium groups. The colored anions of such dye salts may be, for example, the ions of dye carboxylic acids or, more advantageously, of dye sulphonic acids or of complex metal compounds of metallizable dyes consisting of one equivalent of trivalent co-ordinative 6-valent heavy metal, particularly chromium or cobalt, and of two equivalents of dyes forming bicyclic metal complexes, for example, of the class of o,o'-dihydroxyor o-hydroxy-o carboxy-azo or azomethine dyes.

Suitable colorless cations in these salts are the cat ions of primary, secondary or tertiary organic amines of the aliphatic, cycloaliphatic, araliphatic, aromatic or heterocyclic series or of cyclic amines. Suitable colorless anions in soluble salts are particularly the residues of organic acids, and particularly of aromatic sulphonic acids, for example anions of alkyl-alkoxy-benzene sulphonic acids. Suitable salts of colored cations with colored anions, which salts are soluble in organic solvents, may be, for example, the precipitation products of dior triphenylmethane dyes or of rhodamine dyes, which may contain sulphonated chromium or cobalt complexes of o,o-dihydroxyor o-hydroxy-o'-carboxy-azo dyes.

Optical brightening agents of the known classes, such as, for example, 7-diethylamino-4-methylcumarin or 7-dimethylaminocumarin or 7-monoethylamino-4- methylcumarin are also suitable processing agents.

Furthermore, the following agents may be used for the processing:

Waterand oil-repellant making agents, such as fatsubstituted aminoplastics, polyamides containing chlorhydrin groups, silicones, carboxylic acid perfluorides and chromium salts thereof, antistatic and dirt release agents, such as phosphoric acid esters of fatty alcohols and polyethylene glycol, flame-proofing agents, such as aminoplastics and phosphorus compounds, agents for the preservation of textiles against rotting, such as chlorinated phenol derivatives and copper salts thereof, anti-shrinkage and anti-matting finishes for wool, such as melamine and epoxy resins, and crease resistant making agents, such as aminoplast formers containing methyl groups.

One or more of the aforementioned agents may be used for the processing carried out subsequently to the dyeing process.

The invention is preferably applied to the dyeing of textiles, dyeing being for this reason hereinafter solely referred to.

The organic solvents used for the dye liquor, particularly hydrocarbon halides, such as perchloroor trichloroethylene, are highly volatile even at normal temperature. ln dyeing processes in which an organic solvent of this kind is the essential constituent in the liquor, a substantial proportion of the solvent used is generally in the gaseous state above the fluid in the containers containing the dye liquor, this being due to the heating during the dyeing process. This involves not only losses and undesirable excess pressures, but when a substantial proportion of the solvent has evaporated from the liquor, the quantity and composition thereof no longer correspond to those of the original mixture. This change in quantity and composition of the liquor involves the risk of non-homogeneous dyeing conditions changing in an uncontrollable manner being obtained and thus the possibility of varying depths of color of the textiles to be processed being obtained.

OBJECTS OF THE lNVENTlON It is thus an object of the invention to remove these disadvantages and to create dyeing conditions which are as constant and positive as possible so that constant dyeing results may be obtained. The invention is based on the fact that it is an essential prerequisite to constant dyeing conditions that a constant ratio in the liquor is maintained, that is to say that the quantity of solvent in the liquor upon termination of the treatment should correspond exactly to the quantity present therein at the beginning of the treatment. In a narrower sense, it is thus an object of the invention to maintain the ratio in the liquor constant, that is to say to maintain the ratio of volume of liquor to the weight of the treated goods constant. It is a further object of the invention to ensure a substantial constancy of the composition of the liquor. This includes, for example, that undesired water, which may have been absorbed from the textiles, is continuously removed from the liquor in order to ensure that the liquor reaches its peak boiling point during the dyeing process. The risk of an excess pressure resulting from the evolution of gas in the plant has also to be avoidedv SUMMARY OF THE INVENTION In accordance with the invention, this problem is solved in that the gas evolved by evaporation is at least partially withdrawn from the liquor during the dyeing process, (that is to say, during the processing in general) and condensed upon the supply of heat, the solvent constituent in the condensate thus obtained being returned to the liquor with or without the water constituent, that is to say the continuously formed condensate is instantaneously returned to the liquor. By this measure it is thus ensured that the quantitative ratio in the liquor-dye-textile fiber system remains substantially constant and correspondingly constant dyeing conditions thus prevail during the whole period of the treatment. Since the evolving gas is continuously condensed, an undesirable excess pressure can be avoided. It is even possible to operate the plant under atmospheric pressure.

In accordance with the invention furthermore, not only the quantity of solvent, but also the amount of water present in the system, which forms an azeotropic mixture with the solvent, is maintained constant by returning the condensate to the liquor without decomposition thereof into its phase. This is particularly important wherever the water plays a quantitative part in the dyeing process. The dyeing conditions remain constant, since the correct quantity of evaporating mixture of solvent and water is returned to the liquor. Where the water constituent is of no importance or even undesirable and originates solely from the actual textiles, it may, in the case of a dry solvent being used, be discharged together with condensed solvent through a water separator in which the water is removed, whilst the solvent is, in accordance with the invention, returned to the liquor. In accordance with the invention, where it is of importance that the water constituent should be present in the liquor in an emulsified form, the undercomposed condensate may be passed through a pump or a corresponding emulsifier before it is returned to the main liquor, the condensate being introduced into the liquor after the water constituent present in the condensate has been sufficiently finely dispersed in the solvent by the pump. In dyeing processes, in which the liquor is heated, the gas pressure generated is, in accordance with the invention, adjusted to a determined value by an adjustable excess-pressure safety device and/or by regulating the cooling capacity of a condenser in which the rising vapor is condensed.

One particularly advantageous measure taken in a development of the invention consists in that, subsequent to the removal of the dye liquor, that is to say before the dyed textiles are removed from the dyeing apparatus, the dyed textiles are dried by air circulation until the solvent constituent present therein has been extensively removed and condensed, whereupon the air circulation can be stopped irrespective of the water constituent still present in the dyed material. The air circulation thus has not the purpose of drying the dyed textiles completely, its purpose being merely the recovcry of residual solvent still present therein.

Where the dyeing is carried out in the presence of water with the water serving as the medium carrying the dye to be applied to the textiles, the liquor frequently contains electrolytically active additives, such as salts, acids or bases which, when the liquor has been drained, still adhere to the fiber upon termination of the dyeing process and have to be removed by rinsing. Where an organic solvent is used which thus forms the main operating medium, in which the water carrying the dye, for example in the form of an emulsion, is carried to the fiber, such electrolytic additives cannot be removed by rinsing with a solvent, since they are insoluble therein. In accordance with the invention therefore, where an organic solvent of this kind is used for dyeing, the liquor is drained from the dye vessel for distillation and the dye vessel still containing the textiles moist with solvent and water, is filled with water so that the dyed textiles are completely immersed in water. The liquor in which the dyed textiles are rinsed thus consists of water which, when heated, forms an azeotropic gaseous mixture with the remaining residues of solvent. During heating, the quantity of evaporating solvent exceeds substantially the quantity of evaporating water, so that the solvent residues still remaining in the water-soaked textiles can be recovered by condensation and only water thus remains in which the dyed textiles can be thoroughly rinsed without the loss of solvent. The moment at which the solvent has been extensively recovered can easily be determined through a flow inspection window or may be determined with the aid of a flow meter of known construction through which the condensed solvent flows after the water constituent has advantageously been removed therefrom in the water separator.

Apparatus for carrying out the method according to the invention comprises at least one dye vessel, in which textiles or the like are received, and a pipeline system with pump for conveyance of the dye liquor. In accordance with the invention, the vessel may on principle be provided in any suitable form. Thus, any known dyeing apparatus, for example in the form of a beam, a jigger, a drum, a paddle vat (I-Iaspelkufe), a dyeing star, or the like may be used. In apparatus of this kind, the essence of the invention consists in the dye vessel being connectable by a conduit to a condenser the condensate outlet of which is connectable to the dye vessel. With the aid of these additional features, the solvent vapors rising in a dyeing machine may be intercepted and condensed during the whole period of dyeing. All of the condensate, or at least the solvent phase thereof, may then be returned continuously to the liquor.

In accordance with the invention, instead of connecting the condensate outlet directly to the vessel, it may also be connected to the suction side of the pump whose pressure side is connectable to the dye vessel. This measure is particularly advantageously applied when the water constituent in the condensate is to be emulsified in the solvent. The suction side of the pump is advantageously adapted to be connected to the vessel for the purpose of circulation of the liquor.

In one development of the invention, the apparatus according to the invention may be modified and varied in many ways. Thus, for example, in addition to the actual dye vessel, further vessels containing heated dye liquor may be so constructed as to be connectable to the condenser, so that no excess pressure is generated in these additional vessels. Furthermore, the end of the condenser opposite the gas inlet may be in communication with the outside atmosphere, preferably through a pressure relief valve, so that the dyeing may be carried out at any desired gas pressure, even at atmospheric pressure, without the loss of solvent. It is particularly advantageous for the cooling capacity of the condenser to be adjustable in dependence upon the gas pressure in the dye vessel.

In one particularly advantageous modification of the invention, the dyeing apparatus is a dry-cleaning machine, in which the condensate outlet of the condenser which is connectable to the cleaning drum, can be connected not only to a water separator as hitherto, but also to the drum housing either directly or through a pump. Machines of this kind can thus be used for a new purpose, that is to say, for dyeing, in the course of a manufacturing process. In the process according to the invention a continuous condensation takes place not only during the drying of the textiles, but particularly when the drum contains the heated liquor for dyeing, and the recovered condensate is returned to the liquor, whereas in the conventional operation of machines of this kind, parts contacting the dye liquor are made of a correspondingly resistant material, for example stainless steel. The use of machines of this kind affords the additional advantage that, whereas in the convention dyeing devices the textiles have to be removed or withdrawn from the dye vessel proper in order to be centrifuged and dried, all of these treating processes can now be carried out in the same container, namely in the drum of the machine.

DESCRIPTION OF THE DRAWING These features and further features of the invention are diagrammatically illustrated by way of example in the accompanying drawings, in which:

FIG. I shows a diagram illustrating the basic idea underlying the invention;

FIG. 2 shows a dry-cleaning machine adapted to the purposes of the invention;

FIG. 3 shows a further example of dyeing apparatus with dyeing drum;

FIG. 4 shows a modification of FIG. 2; and

FIG. 5 shows laboratory dyeing apparatus.

SPECIFIC DESCRIPTION In FIG. I, a dye vessel l which, as previously mentioned, may be of any suitable construction, is connected by a conduit 2 to the inlet of a condenser 3. The condensed solvent collects at the lowermost position 4 of the condenser housing and flows off through a conduit 5. According to whether valve 6 or valve 7 is in the open position (one or the other valve being then closed), the condensed solvent returns either directly through conduit 11 or through pump 8 and

conduits

13,12 and 11 to the dye vessel 1, in which the dyeing process takes place. The condenser may be evacuated to the outside through a line 9. In order to obtain a determined operating pressure, the evacuation proceeds through a pressure relief valve 10 provided in line 9, the valve being adjustable to a desired operating pressure. The valve 10 may be omitted when the work is performed only under atmospheric pressure.

FIG. 2 shows an embodiment of the invention in the form of a solvent-dyeing installation evolved from a dry-cleaning machine, in which the textiles may be dried after completion of the dyeing process. An air shaft 22 extends from a drum housing 1 in which a rotatable drum filled with textiles is mounted, through a ventilator 159 to the inlet of a condenser 3 containing heat exchangers 3' for the condensation of the inflowing solvent vapours. The air shaft 21 extends from the outlet of the condenser 3 through an air heater back to the drum housing 1 Branching off from the condensate outlet 2,5 of the condenser 3 in addition to a conduit extending through valve 16 to a water separator (not shown) are conduits 13 and 11 through

valves

7 and 6 respectively, the conduit 13 being connected to the suction side of pump 8 and conduit 11 being connected directly to the drum housing 1'. The additional conduits I1 and 13 are normally not required in drycleaning machines.

The solvent gas can be fed to the condenser through the air shafts generally provided in cleaning machines. Where a vent duct extending into the open is available, it is merely necessary to provide flaps or the like in order to ensure that the solvent gases flow into the heat exchanger of the condenser instead of flowing into the vent duct.

In the embodiment illustrated in FIG. 2, a special connecting line 2 extending from the drum housing 1 directly to the inlet of the condenser is provided for carrying out the process of the invention. For this purpose, the

air shafts

22 and 21 in the zone of the drum housing 1 may be closed by adjustable shutters 17 and 18 during the dyeing process. In addition, the inlet and outlet of the housing of the condenser 3 may be closed by

shutters

23 and 24 so that the ventilator 9 and the air heater 20 do not contact solvent vapours except when they are in operation. The provision of a special connecting line of this kind constitutes a development of the invention. By obturation of the air ducts, that is to say by separation of the air ducts from the drum housing and from the condenser and by the provision of conduit 2 a controlled condensation in the heat exchanger 3 is obtained and undesirable accumulations of residues of condensed solvent or water in the air circulation system are avoided. The conduit 2 may be basically dispensed with when the available air shafts, or one thereof, are or is used for feeding the solvent gases to the condenser.

The vent duct 9 extending from the condenser housing into the open may be closed by a shutter 25 during circulation of the air upon subsequent drying. The dyeing process may thus be carried out under atmospheric pressure with the shutter 25 in the open position; however, in order to avoid loss of solvent, the cooling capacity of the condenser 3 has to be sufficient to ensure that all of the solvent entering in the gaseous form is condensed.

The conduit 2 extending from the drum housing 1', or from the dye vessel 1 in general, to the condenser 3 contains a pressure relief valve 27 by which the desired operating pressure in the drum housing 1 or in the dye vessel 1 is adjustable. In this case, the condensate is passed through the pump 8, a non-return valve 27a being advantageously provided in the conduit 13 on the suction side of the pump. The solvent then flows from the pressure side of the pump through

conduit

12,12a and 11 to the dye vessel. Instead of the valve 17, a pressure relief valve may also be provided in the vent duct 9 as provided in FIG. 1. These valves are omitted when the work is to be carried out under atmospheric pressure. In addition, a pressure meter 71 is provided by which the pressure in the dye vessel or drum casing l is measured and the supply of coolant 72 to the heat exchanger 3 of the condenser 3 is controlled in dependence upon that pressure.

The

conduit

12, 12a and l 1 together with the conduit section 26 connectable to the outlet of the drum housing 1 and to the suction side of the pump, are used for recirculation of the liquor during the dyeing process as is generally the practice. By adjustment of the appropriate valves, the circulating liquor may be caused also to flow through a filter 28. The reference numeral 29 denotes a distillation vessel, the reference numeral 30 denoting a solvent reservoir from which the solvent, to which the dye has to be added, is filled into the drum or drum housing through a pump 8 and conduits l2, and 12a. A coarse filter 31 is provided upstream of the pump 8 for its protection. The drum housing 1' is provided with a steam jacket 32 for heating the liquor. The liquor may be preheated optionally in one of the pump lines by a suitable intermediate heat exchanger.

FIG. 3 shows a dyeing machine, in which a dyeing drum rotating in a drum housing is also used. Those parts of the plant the function of which corresponds to that of corresponding parts in FIGS. 1 and 2 are de noted by the same reference numerals. The conduits carrying predominantly fluid are shown in full lines, whereas the lines carrying gases and vapors are, in this construction, indicated by dotted or broken lines in order to facilitate understanding.

In this construction also, the solvent vapor and water vapor, according to the method employed, evolved in the drum housing 1' pass through conduit 2 to the inlet of the condenser 3 when the shut-off valve 33 and the pressure relief valve 27 are in the open position. The condensate flowing off through conduit 5 is fed either to the liquor in the drum housing 1 or to the suction side of the pump 8, or to a water separator 34, according to whether

valve

6,7 or 16 is in the open position. The feed to the pump 8 takes place when the water constituent present in the condensate has to be present in emulsified form in the liquor. As a result of the vigorous mechanical movement of the condensate in pump 8, the water constituent in the solvent is very finely dispersed and can thus be returned to the liquor in the drum housing 1 through the

conduits

12, 12a and 11. The water constituent may, however, also be separated from the solvent by feeding the condensate to the water separator 34. This measure is required whenever the water constituent in the system has to be removed in order to ensure that the pure solvent reaches its boiling point upon pressure-less operation. During the dyeing process, the pure solvent is then returned from the water separator 34 to the liquor in the drum housing I through a valve 35, the valve 36 being then closed. Conversely, during the subsequent drying process for recovery of the solvent still present in the dyed textiles, the valve 35 is closed and valve 36 is open. The quantity of solvent condensed per unit time is then ascertained by means of a flow meter 37 and the drying time required is thus determined. Alternatively, the termination of the drying period may be ascertained by watching the flow of solvent through an inspection window 69.

The chemical additives are prepared in a container 38. The solvent from a reservoir 30 is introduced by the pump 8 into the container 38 through conduits 3S, 40, 41 (with the

valves

42, 43 and 44 in the open position), the dye and any water used being introduced by opening a cover 45. For thorough mixing of the liquor, the container 38, in which the dye mixture is prepared, is provided with a stirrer 46 and a steam jacket 47 for heating the liquor. The valve 419 is opened and the tinished liquor mixture flows through conduit 48 to the pump 3 be to fed thereby either through conduits 419 and 50 to the liquor reservoirs 51 and 52 (the valves 43 and 53 as well as valve 49 being then open) or through

conduits

12, 12a and 11 (the valves 49 and 54 being then open) to the drum housing 1' which contains the textiles to be dyed.

During the subsequent dyeing process, the textiles in the liquor in the drum housing 1 are moved mechanically by the drum, the solvent vapours rising from the heated liquor being continuously condensed and returned to the liquor in the manner hereinbefore described. Simultaneously, the liquor is recirculated by the pump 8 through the

conduits

26, 112, 12a and H. The

valves

55 and 54 are then in the open position. For recirculation through the filter 23, the

valves

56 and 57 instead of the valve 54, are opened. The quantity of liquid in the drum housing 1' is indicated by a liquor level indicator 58. Finally, the liquor is pumped by the pump 8 from the drum housing I to the distillation vessel 29 (the

valves

55 and 59 being then open), into which vessel the content of the filter 28 may also be drained, or the liquor is pumped back to one of the reservoirs Si or 52. When the solvent used has drained from the drum housing, the textiles are centrifuged (it will be appreciated that this is impracticable in stationary dyeing apparatus) and the solvent obtained is also pumped off. In a water separator 61, the solvent constituent, separated upon distillation from the condensate in the condenser 60, is fed through conduit 62 to the reservoir 36.

In certain dyeing processes, the drum housing is then filled with water by opening a valve 63 of a water main 64 entering from without. The textiles present in the drum are rinsed in this aqueous rinsing liquor by turning the drum. Simultaneously, the rinsing liquor is heated to the azeotropic boiling point by charging the steam hacket 32 with steam, so that the solvent residues present in the rinsing liquor and originating from the textiles evaporate and can be returned to the tank 30 after condensation in the condenser 3 and separation in the water separator 34. Only then is the rinsing liquor removed from the drum housing ll through conduit 65. The articles from which the solvent has been lid removed and which are only moist with water, are finally centrifuged and may then be withdrawn from the drum housing. The textiles are then ventilated by opening a fresh-air flap and the dry textiles can then be removed from the dyeing apparatus. However, when no water has been poured into the drum, the shutters 23 and 2d are opened and a stream of warm air is passed with the aid of a ventilator 119 and an air heater 20 through the drum housing 11 and through the air shafts 231 and 22 while the solvent vapors entrained by the air current from the drum housing I are condensed in the condenser 3 and fed to the water separator 34 until the flow of solvent in flow meter 37 is below a determined minimum value. The

air shafts

21 and 22 are connected to the drum housing 1, as is the case in FIG. 2. in H6. 3 the said shafts are shown only partially for the sake of easy surveyance.

In the construction illustrated in FIG. 3, the vessel 38 in which the dye is prepared, and the coarse filter 31, both of which contain portions of the dye liquor, may be connected by additional conduits 67 and 69 to the condenser for recovery of the solvent vapours escaping from the liquor. Similarly, the

liquor reservoirs

51 and 52 may, if necessary, also be connected by such additional connecting lines to the inlet of the condenser, for example when the liquors in

reservoirs

51 and 52 are to be preheated. In the construction illustrated in FIG. 3, as in the construction illustrated in FIG. 2, means for measuring the pressure in the drum housing 1' by which the supply of coolant to the heat exchanger 3 of the condenser may be controlled in dependence upon the measured pressure, may be provided.

FIG. 4 shows a modification of FIG. 2 which is distinguished from the construction shown in FIG. 2 by the connecting line 2 being connected to the condenser 3 or heat exchanger 3' on the opposite side thereof, that is to say, in the zone of the condenser outlet. This makes it possible to dispense with the shutters for closing the condenser inlet and outlet and for cutting off the air circulation system. An undesired recondensation of the solvent in the air shaft 21 is prevented by the evolution of heat in the air heater 20, in which solvent is removed from the gases passing through the heat exchanger 3', so that the air still present on the other side of the heat exchanger can escape through the additional vent duct 9 connected to the vent duct 9, the additional vent duct 9' containing an adjustable pressure relief valve MI. The further component parts of the plant not shown in FIG. 4 correspond to those in FIG. 2 and are thus not shown in order to ensure easy surveyance of the drawing.

FIG. 5 shows a construction particularly suitable for laboratory purposes. This construction comprises (1 a rotatably mounted flask extending at an angle and provided with recesses; (2) a reflux condenser above the flask; (3) a solvent reservoir opening out through a dosing or apportioning device into the reflux condenser; (4) a suction tube having a flexible end opening out into he flask through the neck thereof, and on the other side opening out into a reservoir which can be connected to a vacuum line, and (5 a distributor by which the solvent dropping from the reflux condenser may be fed into a supply flask for pure solvent and which allows the vapor to flow from the flask into the reflux condenser.

The dye vessel, hereinafter briefly referred to as a dye flask, is provided with inwardly extending recesses for the purpose of forcing the dyed textiles to carry out a discontinuous movement. The recesses prevent the textiles from continuously following the rotation of the flask. The dyed textiles initially adhere to the recesses to fall eventually from the inwardly extending projection to another position of the wall of the flask as the flask continues to rotate. The dyeing apparatus is advantageously made of glass. The flask may be heated by a heating bath into which the flask dips. The rotational movement about an axis turned through an angle of about 20 to the horizontal, is advantageously pro duced by known devices, such as rotary evaporators, which simultaneously afford the advantage of being provided with a heater.

The construction shown in FIG. is as follows:

A is the dyeing flask provided with scoop-shaped re cesses;

B is a rotary device consisting of a commercially available evaporator;

C is a heatable container for dye additives, such as dye preparations and the like, provided at the bottom with a filter and a cock;

D is a dosing or apportioning vessel;

E is a collecting vessel for used solvent;

F is a collecting vessel for pure solvent;

G is a heating bath with thermostat;

H is a solvent reservoir;

I is a feed hopper;

K is a distributor;

L is a suction tube having a flexible end;

M is a pump;

X,Y are condensers or coolers;

V ,V are suction lines, and

A,K are absorption vessels.

In accordance with the invention, the textiles to be dyed are treated with a constant quantity of liquor of a constant composition and thus under substantially constant dyeing conditions. Undesired water constituents can be removed. Undesired excess pressure is avoided. Th extent to which the textiles are subjected to mechanical stresses is substantially constant owing to the constant quantity of the liquor. The use of drycleaning machines affords the further advantage that not only the rinsing, but also the drying of the dyed textiles can be carried out in one and the same container. The invention affords the further advantage that under a constant pressure the required dyeing temperature can be obtained, since the water constituent can be readily removed or may be maintained at a constant value, this having hitherto been impossible in the conventional completely closed systems, such as HT- dyeing machines. In addition to affording the advantages of constant operating conditions, the apparatus according to the invention may be of a relatively cheap construction, since no pressure vessel is required. As mentioned previously, the container containing the dyed textiles and the liquor need not necessarily be provided in the form of a dyeing drum, but may be of any other known construction, for example an HT- dyeing machine, a paddle vat (Haspelkufe) or jigger, a coil-former or beam type dyeing appartus or the like. The invention is thus not limited to the illustrated constructions.

In the following examples, the parts, unless otherwise indicated, are parts by weight, the percentages are percentages by weight, the temperatures are given in centigrades, and the numerals and capital letters relate to FIG. 5.

Specific Examples EXAMPLE 1 parts of a polyester tricot fabric (DiolenLoft tricot) are dyed with 2.4 parts of a dispersion dye of the following formula dissolved in 480 parts of perchloroethylene and further 2,720 parts of perchloroethylene as follows:

Cock 2 is closed, cock 1" is opened. The container D is filled with 2,720 parts of perchloroethylene, and the textile is then put into flask A. The cocks 5" and 6" are closed and cock 4 is opened, so that the perchloroethylene may flow into flask A. The oil bath G is then heated to The intermittent rotary motor B, which changes its direction of rotation, is then started (30 seconds in each direction of rotation, 15 seconds stationary).

Cock 8" is then closed and 2.4 parts of dispersion dye and 480 parts of perchloroethylene are introduced into flask C. In flask C, the solution is brought to the boil by means of a heater (not shown in the drawing), whereby the dye goes into solution. Cock 8 is opened and the solution is introduced into flask A through a filter provided at the bottom of vessel C. The dyeing is carried out for a period of 45 minutes.

The oil bath G is then removed, cocks 4", 6 and 8" are closed and cock 5" is opened. The apparatus is emptied through suction line V and the dye liquor flows into flask E.

For the after-treatment, the material is washed in the same flask with a mixture of perchloroethylene and a cleaning intensifier of the kind generally used in drycleaning, that is to say for 15 minutes at 50. The rinsing is effected with a pure solvent for 5 minutes at 2030.

For the drying, the cocks, 2", 5", 8" and 9" are closed, cocks 3" and 6" are opened, and the apparatus is evacuated through suction line V Flask A is heated to a temperature of 80, so that the solvent in flask A evaporates very quickly. The vapours, condensed in condenser X, flow into container F. The fabric is dry when the solvent discontinues to distill over. Cock 3" is then closed. The vacuum in the apparatus is slowly overcome by the air flowing in through cock 5". Flask A is then disconnected from the attachment H and the dyed, dry piece of tricot can be removed from the flask. A uniformly pink colour is obtained.

Regeneration of the solvent: Flask E instead of flask A is connected to the distributor K and the procedure is then the same as upon drying. The pure solvent collected in vessel F can be returned the reservoir H by pump M.

EXAMPLE 2 The method employed in Example 1 is applied except that the material consists of polyamide socks (100 parts), 3 parts of dye of the formula and 3,680 parts of perchloroethylene. A uniformly blue colour is obtained.

We claim:

1. An apparatus for the treatment of textiles, comprising:

a textile-treatment container receiving the textiles to be treated in a treating liquor including a volatile solvent immiscible with water and having a specific gravity greater than that of water, said liquor also including water dispersible in said solvent;

a condenser having a vapor inlet connected to said container above the liquor therein, and a condensate outlet;

a pump having a suction side directly connected to said condensate outlet, and a pressure side connected to said container for agitation of the liquor therein; and

conduit means connecting said suction side of said pump with said container directly to form a liquidcirculation path including said pump and said contain'er.

2. An apparatus for the treatment of textiles, comprising:

a pump having a suction side directly connected to said condensate outlet, and a pressure side connected to said container for agitation of the liquor therein;

conduit means connecting said suction side of said pump with said container directly to form a liquidcirculation path including said pump and said container; and

valve means for selectively connecting said condensate outlet and said conduit means to said suction side of said pump each to the exclusion of the other and for selectively directly connecting said condensate outlet to said container and said suction side of said pump.

3. The apparatus defined in claim 2, further comprising at least one processing-liquid receptacle connected to said container.

4. The apparatus defined in claim 2, further comprising a pressure-relief valve connected to said condenser and communicating, upon opening of said valve, with the atmosphere.

5. The apparatus defined in claim 2, further comprising an air-circulation system connected to said container, said aircirculation system including a first airshaft opening into said container, a ventilator connected to said first air shaft, an air cooler connected to said ventilator for receiving air therefrom, a second air shaft connected to said cooler for returning air to said container, and a heater along said second air shaft for reheating air returned to said container.

6. The apparatus defined in claim 5 wherein at least one of said air shafts communicates between said condenser and said container, said air shafts being provided with closure means for obtuating unused sections of the respective shafts.

7. The apparatus defined in claim 5, further comprising shutter means in said air shafts for selectively blocking same.

8. The apparatus defined in claim 5 wherein said cooler has a condensate outlet selectively connectable to a water separator or to said pump.

3 UNITED STATES PA'IENTV OFFICE I CERTIFICATE OF CORRECTION Patent No. 3,783,650 Dated 19 February 1974 Inventor-(s) Hans-Peter WEBER ET AL It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:

' In the heading, line 73', for the Assignees read: I

--CIBA Ltdl, Basel Switzerland andanus, BOHLER' arid I WEBER KG Maschin enfabrik Augsburg} Germany- 1 Signed and sealed this-,llrth day of May-197k,

' 3 (SEAL) Attest:

EDWARD M.FLETCHER, JR C MARSHALL DANN I Attesting Officer Commissioner of Patents

Claims

2. An apparatus for the treatment of textiles, comprising: a textile-treatment container receiving the textiles to be treated in a treating liquor including a volatile solvent immiscible with water and having a specific gravity greater than that of water, said liquor also including water dispersible in said solvent; a condenser having a vapor inlet connected to said container above the liquor therein, and a condensate outlet; a pump having a suction side directly connected to said condensate outlet, and a pressure side connected to said container for agitation of the liquor therein; conduit means connecting said suction side of said pump with said container directly to form a liquid-circulation path including said pump and said container; and valve means for selectively connecting said condensate outlet and said conduit means to said suction side of said pump each to the exclusion of the other and for selectively directly connecting said condensate outlet to said container and said suction side of said pump.
3. The apparatus defined in claim 2, further comprising at least one processing-liquid receptacle Connected to said container.
4. The apparatus defined in claim 2, further comprising a pressure-relief valve connected to said condenser and communicating, upon opening of said valve, with the atmosphere.
5. The apparatus defined in claim 2, further comprising an air-circulation system connected to said container, said aircirculation system including a first air-shaft opening into said container, a ventilator connected to said first air shaft, an air cooler connected to said ventilator for receiving air therefrom, a second air shaft connected to said cooler for returning air to said container, and a heater along said second air shaft for reheating air returned to said container.
6. The apparatus defined in claim 5 wherein at least one of said air shafts communicates between said condenser and said container, said air shafts being provided with closure means for obtuating unused sections of the respective shafts.
7. The apparatus defined in claim 5, further comprising shutter means in said air shafts for selectively blocking same.
8. The apparatus defined in claim 5 wherein said cooler has a condensate outlet selectively connectable to a water separator or to said pump.