US3797997A

US3797997A - Method for fixing the shape of textile materials

Info

Publication number: US3797997A
Application number: US00084251A
Authority: US
Inventors: H Feldtman; B Fleischfresser
Original assignee: Commonwealth Scientific and Industrial Research Organization CSIRO
Current assignee: Commonwealth Scientific and Industrial Research Organization CSIRO
Priority date: 1969-11-06
Filing date: 1970-10-26
Publication date: 1974-03-19
Anticipated expiration: 1991-03-19
Also published as: DE2054159A1; GB1330705A

Abstract

Textile materials consisting of or containing wool or other keratinous fibres are maintained, without external restraint, in a cohesively set configuration by depositing on the materials a substance that renders the materials resistant to loss of cohesive set during subsequent treatments to establish permanent set in the material.

Description

United States Patent [1 1 Feldtman et a1.

METHOD FOR FIXING THE SHAPE OF TEXTILE MATERIALS Inventors: Henry Douglas Feldtman, Point Lonsdale; Barry Edwin Fleischfresser, Belmont, Victoria, both of Australia Commonwealth Scientific and Industrial Research Organization, Melbourne, Victoria, Australia Filed: Oct. 26, 1970 Appl. No.: 84,251

Assignee:

Foreign Application Priority Data Nov. 6, 1969 Australia...'. 63436/69 May 14, 1970 Australia 1207/70 US. Cl 8/I27.6, 8/128 R, 8/128 A,

8/D1G. 11, 38/144 Int. Cl... 006m 3/10, D06m 3/06, D06m 15/16 Field of Search 8/127.5, 127.6, 128, DIG. 11

References Cited UNITED STATES PATENTS 7/1963 Reider 8/127.6 2/1970 Farmer et a1. 8/l27.6 3/1970 Cain 8/1276 2/1972 Delmonico et a1. 8/128 Cook et a1., Textile Institute and Industry, September, 1969, pp. 247-248.

Kopke Journal of the Textile Institute, 61 (8) 361-387 (1970) Feldtman et a1., Textile Institute and Industry, September, 1970, pp. 249-252.

Angliss et 211., Applied Polymer Symposium, No. 18, 1027-1043 (1971).

Primary Examiner-George F. Lesmes Assistant Examiner-J. Cannon Attorney, Agent, or Firm-Stowell & Stowell 5 7] ABSTRACT Textile materials consisting of or containing wool or other keratinous fibres are maintained, without external restraint, in a cohesively set configuration by depositing on the materials a substance that renders the materials resistant to loss of cohesive set during subsequent treatments to establish permanent set in the material.

6 Claims, No Drawings METHOD FOR FIXING THE SHAPE OF TEXTILE MATERIALS This invention relates to an improved method for rendering the configuration of textile materials substantially resistant to the effects of machine laundering for the life of the material.

In particular, the invention relates to a method for maintaining the cohesively set configuration of such materials, without external constraint, during subsequent setting and stabilising treatments.

The textile materials, with which this invention is concerned, may be in the form of fibres, yarns, fabrics or garments, and the term *materials" as used in the following description, is to be understood as including all such forms.

The present invention is concerned with the treatment of materials consisting of or containing wool or other keratinous fibres, that is fibres which contain disulphide linkages capable of rearranging under certain conditions.

' It is known, that in order to fix materials containing wool or other keratinous fibres flat or in creases, pleats, or other desired configuration, so as to withstand change in shape during a series of complete laundering cycles (machine washing and tumble drying), it is necessary to treatthe said'materials by any of the various methods known to prevent felting, such as by treatment with various oxidising agents in water or salt solutions, various monomers, acid chlorides, reactive chlorine compounds, reactive polymers, etcsln addition, a state of minimum energy must be established in the wool or other keratinous fibres, in their new configuration, through stress relaxation, that is, through rearrangement of a major portion of the cross-linkages and other bonds between the polypeptide chain molecules. In this state there are no internal forces tending to return the fibres to their original configuration. This operation is generally referred to as setting".

During laundering, however, forces applied to the fibres in the set configuration can distort this configuration and further bond re-arrangement can occur. The results of such re-arrangement is the loss of part of the desired configuration. A number of methods are known by which the set configuration can be stabilised and rearrangement of the molecular structure in response to an applied stress inhibited.

The basic requirements for imparting a permanent shape to materials containing wool or other keratin fibres are, therefore, setting (stress relaxation) followed by stabilisation of the set structure. It is also necessary that the materials be rendered non-felting; an operation that can be performed before, after, or simultaneously with setting or stabilising steps.

One method of setting the shape of wool or other keratinous materials in any desired configuration is to restrain the materials mechanically in the new shape and then subject them to a treatment with saturated steam. This operation is commonly carried out in the presence of a reducing agent and water in order to speed up the rate of re-arrangement of the disulphide cross-linkages and other intermolecular bonds, that is, to effect rapid stress relaxation of the fibres through the production of free thiol groups and the well established mechanism of thiol-disolphide interchange. The term temporary set" will be used herein to describe the condition of materials which have been so treated.

Following this temporary setting of the new shape, the materials can be fixed or stabilised, while being held in the desired configuration, to produce what will be referred to as a permanently" set condition of the materials. This may be achieved by various known means, for example, as follows:

a. by steaming with saturated steam in a chamber for 2 to 3 hours;

b. by introducing, with the aid of suitable polyfunctional reagents, an additional network of stable crosslinkages to oppose thiol-disulphide interchange if the fibres are subjected to further stress (as described in co-pending US. Pat. application Ser. No. 877,427 filed Nov. 17, 1969.

c. by removal of free thiol groups by blocking with monofunctional reagents, by oxidation, or by complex ing with divalent metal ions; or i d. by various combinations of the above methods.

When these methods are used commercially to stabilise the desired shape in wool or other keratinous materials, it is an essential requirement that the material is first given adequate temporary set by e.g., steaming in the wet state for at least one minute in the presence of a reducing agent.

In normal garment manufacturing procedures, 15 seconds or less is allotted to steam pre'ssingin order to make the garment attractive and saleable. However, this appearance is immediately lost on wetting the garments with water. Prolonged steam pressing at the garment stage, as required for setting in the presence of reducing agents, creates a bottleneck in processing making it imperative that as short a time aspossible be given to this particular operation. In addition, drying of wet garments adds to the inconvenience and cost of processing.

Various methods of avoiding this bottleneck have been described, e.g. by first steam pressing for less than 15 seconds then hanging the garment in super-heated steam US. Pat. application Ser. No. 58,989 filed July 28, 1970; this method requires that the conditions of temperature and relative humidity be adjusted, so that the cohesive set already introduced is not released, whilst bond rearrangements responsible for temporary and permanent set can still occur, as well as specialised equipment and precise control to prevent loss of the garment shape.

ln the well established practice of forming wool fibres to a desired shape by steaming or heating for l to 10 seconds and then drying and cooling while-holding the shape mechanically, ionic and hydrogen bonds are rearranged but disulphide bonds are unaffected. When wool is in this state, the network of ionic and hydrogen bonds will overwhelm the influence of the disulphide bond network because, even though individually ionic and hydrogen bonds are weaker, their total number offers a much greater and countervailing strength. The new configuration is maintained as long as the moisture content of the fibre is such that sufficient ionic and hydrogen bonds remain intact to exceed the restoring .force due to the disulphide crosslinks. The configuration of wool fibres, yarns and the like due to the rearrangement of ionic and hydrogen bonds, called cohesive set, is lost immediately on wetting. The invention described in co-pending Australian Patent Application 10897/ relies on sufficiently low moisture content during steaming, so that there is insufficient restoring force to release the desired shape when using the procedure described in that invention. it the garments were hung in saturated steam the desired shape would be released immediately.

A principal object of the present invention is to provide a method of maintaining a cohesively set configuration in material consisting of or containing wool or other keratin fibres. This cohesively set shape can then be stabilised and .rendered permanent using steam, under any convenient conditions of temperature and pressure, including saturated steam.

According to the present invention, there is provided a method for maintaining, without external constraint, a cohesively set configuration of a textile material consisting of or containing wool or other keratinous fibres, during a subsequent setting and/or set stabilising treatment, which method comprises the step of depositing on the material a substance that renders the material resistant to loss of cohesive set, said step being carried out before or after a treatment to cohesively set the material.

According to a first embodiment of the invention, the substance which renders the material resistant to loss of cohesive set during a subsequent setting and/or set stabilising treatment, is deposited on the material in its cohesively set configuration under conditions which do not cause loss of cohesive set.

In another aspect of the first embodiment, the invention provides a method for setting a textile material, as defined above, which comprises cohesively setting the material in any suitable manner and depositing on the material in its set configuration an essentially water insoluble substance which renders the material resistant to loss of cohesive set during a subsequent setting and- /or set stabilising treatment, said substance being deposited under conditions which do not cause loss of cohesive set.

In a further. aspect of the first embodiment, the present invention provides a method for permanently set ting a textile material, as defined above, which comprises cohesively setting the material in any suitable manner, depositing on the material in its cohesively set configuration an-essentially water insoluble substance which renders the material resistant to loss of cohesive set during a subsequent setting and/or set stabilising treatment, said substance being deposited under conditions which do not cause loss of cohesive set, and then establishing permanent set in'the material in any suitable manner. I

According to a second embodiment of the method the said substance is deposited on the material and the material is then cohesively set in any suitable manner.

In another aspect of the second embodiment, the present invention provides a method for cohesively setting a textile material as defined above, which comprises depositing on the material a substance that renders the material resistant to loss of cohesive set during a subsequent setting and/or set stabilising treatment, and then cohesively setting the material in any suitable manner.

In a further aspect of the second embodiment, the invention provides a method for permanently setting a textile material as defined above, which comprises depositing on the material a substance which renders the treated material resistant toloss of cohesive set during a subsequent setting and/or set'stabilising treatment, cohesively setting the treated material in any convenient known manner, and finally establishing permanent set in the material in any suitable known manner.

In each embodiment, the substance deposited on the material is preferably a water insoluble, reactive polymer," i.e. a synthetic polymeric material having groups available to react with the material to which it is applied. Alternatively the substance may be one or more pre-polymers or polymer precursors capable of forming such a polymeric material. In either case the polymeric material should be one which does not swell in the presence of water or steam.

Where the substance is deposited on the material which is his cohesively set configuration, the substance must be capable of rendering the material resistant to loss of that cohesive set during subsequent treatment, and also must not destroy that cohesive set when deposited.

Where the substance is deposited on the material before the latter is cohesively set, it is clear that the substance used must not hinder this setting operation in any way-Consequently, the useful substances must be thermoplastic or heat settable at the temperature at which cohesive set is imparted to the material. Accordingly, any substance which meets the above requirements, and is without adverse effects on the character of the material treated, falls within the ambit of this invention.

Specific types of polymers which have been found to be useful in the practice of the invention include:

a. Reactive polyurethanes, i.e. those containing free isocyanate groups. These are typified by Synthappret LKF" and include the following:

Manufacturer Pfcrsee Resin Braxan L 713 +Braxan L 708 +Avivan L 288 Chemical Type SBR containing reactive groups Reactive polyfunctional isocyanatc crosslinking agent residual isocyanate Vibrathane 6006 US. Rubber Do. EP 2923-5 with Ashland lsocyanate prepolymcr catalyst EP 02430l Chemical Co.

Arotap M 520 Ashland lsocyanate prepolymer Chemical Co. Synthappret LKF Bayer Aliphatic lsocyanate prepolymer Braxan LFA Pfersee Do. Lankrothanc I304 Landro Do.

Chemicals b. Reactive polyacrylates, such as Paraloid K7003" (Rohm & Haas Company);

0. Reactive polyolefins, such as Zeset TP" (E1. du Pont de Nemours 8c Co. which is a terpolymer of ethylene, vinyl acetate and methacroyl chloride;

d. Reactive polysulphides, i.e. polymers containing disulphide linkages in the polymer backbone, with thiol side and end groups, typified by Thiokol LP8" and Thiokol LP3" (Thiokol Chemical Corp.); and

e. Reactive poly-(oxyalkylene) resins with attached thiol groups, such as Oligan 474" (Oligan is the registered Trade Mark of Ciba Ltd.)

Good results are obtained when these substances are applied to wool in amounts of from 0.5 to ID percent, based on the weight of the wool.

Before cohesive setting the substance may be deposited on the textile material from solution or dispersion in any suitable liquid medium, e.g. a solution in an organic solvent, such as a dry cleaning solvent, or an aqueous dispersion. However, the establishment of the cohesive set is dependent on the re-arrangement of the ionic and hydrogen bonds and these bonds will be disrupted if the material in its cohesively set configuration is immersed in a polar solvent such as water. Thus where cohesive setting is carried out first, it is preferred that the substance is deposited on the material from a non-polar solvent. Suitable non-polar solvents for use in the process of the invention may be selected from the paraffinic hydrocarbons; chlorinated paraffinic and aromatic hydrocarbons; toluene, benzene, xylene and substituted xylenes.

polyurethanes with blocked isocyanate groups e.g.

Unithune lOOT (Thiokol Chem. Co.)

do. 200 (A do. do. do. 390 CS do. do. do. WS 70 do. do.

Thylon D 406 do. do.

Other substances suitable for use in the modified process of the invention can be made by mixing blocked or masked isocyanates or polyisocyanates in various' Desmodur AP Desmophen v One disadvantage of the process as so far described is that the preferred reactive polymeric materials, e.g. Synthappret LKF, Lankrothane I304, Braxan LFA, readily combine with available water from the surroundings; fabric treated flat with these materials must be stored in a dry atmosphere; This necessitates drying the treated wool. Otherwise, any attempt to store treated fabric in a dry state would be negated by water vapour derived from the wool. This situation is not met with in applying the method of the first embodiment I because, in that instance, the polymer is deposited on the material after the shape has been established.

A similar situation with regard to stability of the useful materials exists with Zeset TP, but in this case the polymer can be heat cured. Therefore, if material carefully treated flat with this polymer is exposed to heat during storage it may suffer a loss of potency with regard to the invention.

This disadvantage can be overcome and other advantagcs gained by a further modification of the basic method. In this modified method the stabilising substances employed have reactive groups which are blocked, i.e. rendered temporarily inactive, but can be reactivated by chemical treatment or heating where required. Typical of such substances and particularly preferred in the practice of the invention are reactive (Polyisocyanate) (polyester modified with saturated low molecular weight fatty acids) (branched polyester containing hydroxyl groups) (branched polyester containing hydroxyl groups) (terephthalic ester containing hydroxyl groups) (terephthalic ester containing hydroxyl groups) (linear polyester containing hydroxyl groups) (Bayer Leverkusen) RD l8 (Bayer Leverkusen) do. 800 do. do.

do. F950 do.

do. l025 do. do.

do. l 700 do. do.

A further aspect of the present invention involves the deposition on the material of a stabilising substance, which not only maintains the cohesively set shape of the material while unconstrained during steaming, but which also renders the material shrinkresistant. The use of such a substance obviates the need to render the material shrinkresistant in a separate operation.

Under suitable conditions, e.g. baking on a hot head press at the appropriate temperature curing of the polymer can be carried out simultaneously with the cohesive setting operation. Thus by choosing a suitable blocked 'polymer cohesive setting, shrink resistance and curing of the polymer may be achieved in a single operational step.

As examples of practical procedures in accordance with the present invention, the following sequences of operations are given; all of which lead to the setting of wool without recourse to prolonged steam pressing of wet material mechanically constrained in the desired configuration.

seousncs l a. treat shrinkresistant material with a stabilising substance;

b. cohesively set the material under conditions where the stabilising substance is thermoplastic;

c. suspend the material in an oven and treat with steam to effect temporary setting;

d. stabilise the set by any of the known methods outlined earlier.

Sequence 2 a. treat shrinkresistant material with a stabilising substance and a setting agent either simultaneously or sequentially;

b. as in parts b,c,d, of sequence 1.

Sequence 3 a. treat material with stabilising substance which also imparts shrinkresistance to the material;

b. as in parts b,c,d, of sequence 1.

Sequence 4 a. treat material with a stabilising substance; which also imparts shrinkresistance, and a setting agent either simultaneously or sequentially;

b. as in parts b,c,d, of sequence 1.

Sequence 5 a. cohesively set shrinkresistant material;

b. treat the cohesively set material with a stabilising substance under conditions which do not cause loss ofcohesive set;

(I. stabilise the set by any of the known methods outlined earlier.

Sequence 6 a. treat shrinkresistant material with a setting agent;

b. cohesively set the material;

c. treat the material with a stabilising substance under conditions which do not cause loss of cohesive set;

d. as in partsc,d of sequence 5.

Sequence 7 a. cohesively set the material;

b. treat material with a stabilising substance which also imparts shrinkresistance to the material, under conditions which do not cause loss of cohesive set;

c. as in parts c,d, of sequence 5. Sequence-8 a. treat the material with a setting agent.

b. cohesively set the material c. treat material witha stabilising substance, which also imparts shrinkresistance under conditions which do not cause loss of cohesive set;

d. as in parts c,d of sequence 5.

The material may be cohesively set in the desired configuration in any suitable manner before the stabilising substance has been deposited; preferably by steam pressing for 2 l5 seconds; When the stabilising substance is applied first, similar conditions may be used, depending on the stabilising substance used. For a reactive polyurethane, the preferred method of establishing cohesive set comprises steam pressing the material in the desired configuration fora period of, for example, 2 15 seconds followed by vacuuming. When the stabilising agent is a reactive polyolefin, such as Zeset Tp, a method of establishing cohesive set comprises pressing the treated material at a temperature of, e.g. 170C for a period of, e.g. 2-60 seconds.

ln carrying out the method of the first embodiment, e.g. Sequences 5 to 8 above, it is often desirable to reinforce the cohesive set initially established by a further short (2 15 seconds) steam pressing operation after application of the stabilising substance and before the 1 final set stabilising operation. This in effect combines the methods of the two embodiments.

Although a principal aim of the present invention, is

to allow the use of steam under any convenient conditions of temperature and pressure to effect permanent setting of a freely hanging garment, the use of unsaturated steam is also within the scope of the invention.

One advantage that can be obtained by the use of saturated steam at atmospheric pressure is that setting, either temporary or permanent, can occur much more rapidly than with the use of unsaturated steam. Also, the use of unsaturated steam in such setting operations on material treated in accordance with the present invention has an advantage that, as the requirements of a stabilising substance for holding a cohesively set configuration in unsaturated steam are less stringent, a wide range of stabilising substances is available for use in maintaining the cohesively set configuration during steaming.

The method of the present invention may be applied to the fixing of fabrics flat, in creases or pleats, and to the fixing of the shape of fibres or fibre structures, such as yarn or knitwear, or any garments such as trousers,

tunics, skirts, cardigans, etc., where dimensional stability is necessary to maintain the appearance of the structure.

The invention is further described and illustrated by the following non-limiting examples.

EXAMPLE l Samples of a grey untreated wool serge material measuring 30 cm X 24 cm were folded to the new dimensions of 30 cm X 12 cm so as to form a crease. These folded samples were placed on the bed of an industrial type trouser press, the press closed,-and a crease insertedin each sample by injecting live steam through the top buck for 2 secs., "baking" for 5 secs. followed by cooling-and drying by applying the vacuum for 5 secs.

Three percent Synthappret LKF, a reactive polyurethane, was then applied to the creased samples from solution in perchlorethylene. After evaporating the solvent, the sampleswere cured for 1 week by storing at 65 percent relative humidity and 20C in a conditioning cabinet provided with a circulating fan.

At the end of the curing period the treated samples were hung, without constraining the crease, in an oven equipped with a thermostat. The temperature in the oven was set at l0OC and after 30 mins. "warm up," live steam was injected at the bottom and the flow maintained for 2 hours to allow the creases to be permanently set and stabilised.

Samples treated in the above manner were given a standard'washing test and the crease retention assessed by comparing the angles formed in yarns at the creases. This testis carried out by extracting yarns from the region of the creases and measuring the angles subtended by each yam near the apex of the crease. Details of the measurements made are given in Appendix I and the relevant results obtained are given in Table l.

EXAM PLE 2 Creases were formed in samples of the grey material as described in Example 1.

Three percent Surlyn T (Zeset), a reactive polyolefin, was applied from solution in perchlorethylene and the solvent evaporated. The treated creased samples were hung in an oven, the creases fixed by injecting steam and then tested as in Example 1. The relevant results obtained are shown in Table l.

' EXAMPLE 3 Creases were formed in samples of the grey serge material as described in Example I.

Three percent of Synthappret LKF was applied from solution in perchlorethylene, the solvent evaporated, and the treated creased samples immediately hung in an oven and the creases fixed by steaming as described in Example 1.

The relevant results obtained are shown in Table 1.

EXAMPLE 4 EXAMPLE 5 Creases were formed in samples of the grey serge material as described in Example 1. Five percent Lankrothane l 304 was applied from perchlorethylene and the samples further treated according to the method described in Example 1.

The relevant results obtained are shown in Table l.

EXAMPLE 6 Creases were formed in samples of the grey serge ma terial as described in Example 1, five percent Lankrothane 1304 was applied from perchlorethylene, and the samples further treated according to the method described in Example 3.

The relevant results obtained are shown in Table 1.

EXAMPLE 7 C reases were formed in samples of the grey serge material as described in Example l. Five percent Braxan LFA was applied from perchlorethylene and the samples further treated according to the method described in Example I.

The relevant results obtained are shown in Table l.

EXAMPLE 8 C reases were formed in samples of the grey serge material as described in Example 1. Five percent of Braxan LFA was applied from perchlorethylene and the samples further treated according to the method described in Example 3.

The relevant results obtained are shown in Table l.

EXAMPLE 9 Creases were formed in samples of the grey serge material as described in Example I. Five percent of Oligan 474 together with three percent of diethylene triamine (on wt of polymer) were applied from perchlorethylene and the samples further treating according to the method described in Example 1.

The relevant results obtained are shown in Table 1.

EXAMPLE l0 Creases were formed in samples of the grey serge material as described in Example I. Five percent of Thiokol LP-3 together with 3 percent of diethylene triamine (on wt of polymer) were applied from perchlorethylene and the samples further treated according to the method described in Example 1.

The relevant results obtained are shown in Table l.

EXAMPLE 1 1 Creases were formed in samples of the grey serge material as described in Example 1. Five percent Thiokol LP-8 together with 3 percent of diethylene triam'ine (on wt of polymer) were applied from perchlorethylene and the samples further treated according to the method described in Example 1. i

The relevant results obtained are shown in Table l.

EXAMPLE l2 Creases were formed in samples of the grey serge material as described in Example 1. Five percent of Oligan 474 together with 3 percent diethylene triamine (on wt of polymer) were applied from perchlorethylene and the samples further treated according to the method 0 described in Example 3.

The relevant results obtained are shown in Table l.

EXAMPLE l3 Creases were formed in samples of the grey serge material as describedin Example 1. Five percent of Thiokol LP-3 together with 3 percent diethylene triamine (on wt of polymer) were applied from perchlorethylene and the samples further treated according to the method described in Example 3.

The relevant results obtained are shown in Table 1.

EXAMPLE l4 Creases were formed in samples of the grey serge material as described in Example li Five percent Thiokol LP-8 together with 3 percent diethylene triamine (on wt of polymer) were applied from perchlorethylene and the samples further treated according to the method described in Example 3.

' The relevant results obtained are shown in Table l.

. EXAMPLE 15 Following the procedure as outlined in Sequence 1 described above:

Samples of a grey serge fabric, measuring 30 cm X 24 cm, were given a shrink-resist treatment using potassium bromate dissolved in common salt solution, ac-

cording to the method described by McPhee McPhee,

J. R. Textile Research Journal 30, 358 1960) These fabric samples were then given a further treatment, using a solution of Zeset TP in perchlorethylene and the excess solution expressed to give a weight increase of 4 percent of the dissolved material. After evaporat- 1 1 ing the solvent, each sample was folded to the dimensions of 30 cm X 12 cm to form a crease. The folded samples were then placed on the bed of an industrialtype hot head press, the press closed, and a crease inserted by pressing for 30 secs with the temperature controlled at 170C. After cooling, the prepared samples were hung without constraining the crease in an oven equipped with a thermostat. The temperature in the oven was set at 100C and after 30 min. warm up, saturated steam was injected at the bottom and the flow maintained for 2 hours to allow the creases to be set and stabilised.

The relevant results obtained are shown in Table l.

EXAMPLE 15 (a) In order to clearly demonstrate the invention, similar samples of the fabric used in Example 15, but without the polymer deposit, were treated as previously described for the use of the polymer.

EXAMPLE 16 Following the procedure outlined in sequence 2 described above:

Samples of a grey serge wool fabric, measuring 30 cm X 24 cm, shrinkresist treated in the manner described in Example 15, were treated in a solution of sodium bisulphite in water and dried to give a weight increase of 2 percent. Four percent of Zeset TP wasthen applied to the flat samples from a solution in perchlorethylene and the solvent evaporated. The samples were then creased, heat set and steamed as described in Example 15, tested as described in Appendix 1, and the relevant results obtained are given in Table l.

EXAMPLE 16 (a) In order to clearly demostrate the invention, similar samples of the fabric used in Example 16, but without a polymer deposit, were given similar treatments to those described with the use of the polymer.

EXAMPLE 17 EXAMPLE 17 (a) In order to clearly demonstrate the invention, similar samples of the fabric used in Example l7, but without a polymer deposit, were given similar treatments to those described with the use of the polymer.

EXAMPLE l8 Following the procedure as outlined in sequence 4 described above:

Samples of a grey untreated wool serge material,

measuring 30 cm X 24 cm, were treated with a solution of sodium bisulphite so as to give a weight increase of 2 percent sodium bisulphite. After drying, these samples were then treated while flat with a solution of Zeset T? in perchlorethylene so as to give a weight increase of polymer equal to 4 percent.

After evaporating the solvent, the samples were creased, heat set and steamed as described in Example 15, and tested as described in Appendix I. The relevant results obtained are as given in Table l.

EXAMPLE 18 (a) Similar samples of the fabric used in Example 18, but without the polymer deposit, were given similar treatments to those described with the use of the polymer.

EXAMPLE l9 Following the procedure as outlined in sequence 3:

Samples of a grey untreated wool serge material, measuring 30 cm X 24 cm, were treated while flat with a solution of Synthappret LKF in perchlorethylene so as to give a weight increase of 4 percent polymer. After evaporating the solvent, each sample was folded to the EXAMPLE 20 Following the procedure as outlined in sequence 4:

Samples ofa grey untreated serge material, measuring 30 cm X 24 cm, were treated with a solution of sodium bisulphite so as to give a weight increase of 2 percent sodium bisulphite. After drying, these samples were then treated while flat with a solution of Synthappret LKF in perchlorethylene so as to give a weight increase of 4 percent polymer. After evaporating the solvent, each sample was folded to the dimensions of 30 cm X l2 cm to form a crease. The folded samples were then placed on the bed of an industrialtype trouser press, the press closed, and a crease inserted by injecting live steam through the top buck for 3 secs., baking for 7 secs., followed by cooling and drying by applying the vacuum for 5 secs. Following the establishment of the creases, the samples were steamed in a chamber as in Example 1, and tested as described in Appendix I.

The following examples show the use of blocked polymers:

EXAMPLE 21 The general procedure followed was as outlined in Sequence 3. The polymer both stabilises and imparts shrinkresistance to the fabric.

i. Samples of a grey untreated wool serge fabric measuring 30 cm X 24 cm were treated while flat withUnithane T, dissolved in ethyl acetate, to give a weight increase of 5 percent of the polymer.

ii. Afterfolding to the new dimensions of 30 cm X l2 cm so as toform a crease, these samples were placed on the bed of an industrial type trouser press, the press closed, and a crease inserted in each sample by injecting live steam through the top buck for 2 secs., bakiii. The treated samples were then cured in an oven for min. at 140C to fix the polymer.

iv. At the end of the curing period the treated samples were hung, without constraining the crease, in an oven equipped with a thermostat. The temperature in the oven was set at 100C and after 30 mins. "warm up," live steam was injected at the bottom and the flow maintained for 2 hours to allow the creases to be set and stabilised.

v. Samples treated in the above manner were given a standard washing test and the crease retention assessed by comparing the angles formed in yarns at the creases. This test is carried out by extracting yarns from the region of the creases and measuring the angles subtended by each yarn near the apex of the crease. The various stages of the treatment at which crease angles were measured are set out above in Appendix I and the results are given in Table l, below.

EXAMPLE 2i (a) in order to clearly demonstrate the invention, similar samples of the fabric used in Example 21, but without a polymer deposit, were given similar treatments to those described with the use of the polymer.

EXAMPLE 22 EXAMPLE 22 (a) in order to clearly demonstrate the invention, similar samples of the fabric used in Example 22, but without a polymer deposit. were given similar treatments to those described with the use of the polymer.

EXAMPLE 23 The general procedure followed was as outlined in Sequence 1.

i. Samples of a grey wool serge fabric measuring 30 cm X 24 cm were given a shrinkresist treatment according to the method described by McPhee (McPhee, J. R., Textile Research Journal 30, 358, (I960) ii. The procedure then followed was as previously detailed in steps (i), (ii), (iii), (iv) and (v) of Example 2l The crease angles measured at various stages of the treatment are given in Table l.

EXAMPLE 23 (a) In order to clearly demonstrate the invention, similar samples of the fabric used in Example 23, but without a polymer deposit. were given similar treatments to those described with the use of the polymer.

EXAMPLE 24 The procedure followed was as outlined in Sequence 2.

i. Samples of a grey wool serge fabric measuring 30 cm X 24 cm were given a shrinkresist treatment according to the method described by McPhee and referred to in step (i) of Example 23.

ii. These samples were then further treated with a solution of sodium bisulphite as described in step (i) of Example 22.

iii. The procedure then followed was as previously detailed in steps (i), (ii), (iii), (iv) and (v) of Example 21. Crease angles measured at various stages of the treatment are given in Table 1.

EXAMPLE 24 (a) in order to clearly demonstrate the invention, similar samples of the fabric used in Example 24, but without a polymer deposit, were given similar treatments to those described with the use of the polymer.

EXAMPLE 25 The procedure followed was as outlined in Example 21, except that curing (step (iii) of Example 2l) was carried out after setting (step (iv) Crease angles measured at various stages of the treatment are given in Table 1.

EXAMPLE 26 The procedure followed was as outlined in Example 22, except that curing was carried out after setting as in EXAMPLE 25 Crease angles measured at various stages of the treatment are given in Table l.

EXAMPLE 27 The procedure followed was as outlined in Example 23, except that curing was carried out after setting.

Crease angles measured at various stages of the treatment are given in Table 1.

EXAMPLE 28 The procedure followed was as outlined in Example 24, except that curing was carried out after setting.

Crease angles measured at various stages of the treatment are given in Table l.

Similar results to those obtained with Unithane T were obtained with Unithane 390CA.

EXAMPLE 29 Five percent of Unithane 2OOCA was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 3 and described in detail in the method of Example 21.

The results are given in Table l.

- EXAMPLE 30 Five percent of Unithane 200CA was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in detail in Table l.

EXAMPLE 3] Five percent of Unithane 390CA was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 3 and described in detail in the method of Example 21. The results are given in Table l.

EXAMPLE 32 Five percent of Unithane 390CA was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

EXAMPLE 33 Five percent of Unithane WS70 was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 3 and described in detail in the method of Example 21. The results are given in Table l.

EXAMPLE 34 Five percent of Unithane WS70 was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table 1.

EXAMPLE 35 Five percent of Thylon D406 was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 3 and described in detail in the method of Example 21. I

The results are given in Table l.

EXAMPLE 36 Five percent of Thylon D406 was applied to samples of a grey untreated wool serge fabric using the general procedures as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table l.

EXAMPLE 37 Five percent of a mixture of Desmodur AP and Desmophen 600 in the proportions of 2:] respectively were applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table 1.

EXAMPLE 38 Five percent of a mixture of Desmodur AP and Desmophen 800, in the respective proportions of 2.511, were applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table l.

EXAMPLE 39 Five percent of a mixture of Desmodur AP and De smophen 1700, in the respective proportions of 2:l, were applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table l.

EXAMPLE 40 EXAMPLE 4l Five percent of a mixture of Desmodur AP and Desmophen F950in the respective proportions of l:3.4 were applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Se quence 4 and described in detail in the method of Example 22.

The results are given in Table 1.

EXAMPLE 42 Five percent of Desmodur AP was applied to samples of a grey untreated wool serge fabric using the general procedure as outlined in Sequence 4 and described in detail in the method of Example 22.

The results are given in Table I.

Table l Crease Crease Crease Crease Example Angle I Angle 2 Angle 3 Angle 4 l 19 22 74 l 2 22 23 76 3 3 26 33 73 29 4 2| 34 72 29 5 28 33 7| 27 6 29 36 66 27 7 32 34 82 29 8 30 33 73 29 9 28 42 62 30 ll) 26 42 6| 33 ll 25 45 78 32 12 26 45 93 33 I3 25 39 9| 3] I4 23 46 87 3S l5 22 33 67 29 I6 20 33 76 28 I7 23 35 72 29 I8 24 29 85 3| I9 28 36 97 42 2O 23 29 7| 30 2| 26 38 H2 22 20 36 86 39 23 23 30 73 23 24 23 29 82 23 25 26 36 I04 42 26 26 35 105 45 27 21 29 63 23 28 22 22 59 22 29 I9 38 78 29 30 I5 3| 82 35 31 I9 34 99 45 32 I6 26 77 35 33 22 39 I05 34 34 I6 24 58 22 35 I8 39 77 42 36 I7 23 58 27 37 I6 35 96 46 38 I8 35 84 38 39 I8 29 62 26 40 I8 36 66 31 41 20 3| 92 34 42 I9 32 77 32 I50 24 56 I33 l6a I9 47 I05 55 l7a 27 68 I65 76 I80 24 55 l29 57 21a 24 68 I65 76 22a 24 55 I29 57 23a 24 56 I33 65 240 I9 47 l05 6O The results as set out in Table I show that a deposit of certain polymers will prevent a change in configura tion of wool fibres during a setting and stabilising treatment in steam. Therefore, this allows a high degree of stability to laundering to be obtained without the need for prolonged steam pressing.

Those persons skilled in the art will appreciate that modifications other than those described above may be made to the process of the invention. The invention includes all such modifications which fall within the spirit and scope.

APPENDIX 1 Measurements of the crease angles were made at various stages in the following manner and the results obtained are as given in Table l.

Crease Angle (l) on dry yarns taken from creases formed in the polymer treated material by the mild steaming treatment in the press and prior to steaming in the chamber.

Crease Angle (2) on dry yarns taken from the crease after steaming in the chamber.

Crease Angle (3) on wet yarns taken after the treated material had been subjected to a 2 hour standard wash test in a domestic washing machine containing a detergent solution maintained at 50C and pH9. These measurements were made on wet yarns floating freely in distilled water at 20C.

Crease Angle (4) on dry yarns taken after the washed samples were tumble dried.

The result shown for measurement (4) is usually less than that shown for (3) because if the crease has an inherent tendency to revert to its original shape, then a pronounced effect will be observed after tumble drying.

We claim:

I. A method of permanently setting woolen textile material which comprises a. establishing cohesive set in the textile material by steaming the material for 2-15 seconds; and

b. applying to the cohesively set material a solution of a synthetic polymer reactive with said material in an organic solvent; or

a impregnating the textile material with an aqueous solution of a synthetic polymer reactive with said material; and

b, cohesively setting the impregnated material by steaming the material for 2-15 seconds; and curing the polymer impregnated material after steps (b) or (b) under heating conditions while the material is without constraint.

2. A method as claimed in claim 1 wherein the polymer impregnated material is permanently set by exposing the material to steam at a temperature of at least 100C for up to 2 hours.

3. A method as claimed in claim 1 wherein the polymer is deposited on the material after cohesive setting thereof, and, following deposition of the said polymer, the material is steam pressed for 2 to 15 seconds to reinforce the cohesive set.

4. A method as claimed in claim 1, wherein said reactive polymer is selected from the group consisting of polyurethanes, polyacrylates, polysulphides, polyoxyalkylene resins with attached thiol groups, polyurethanes with blocked isocyanate groups, and mixtures of blocked isocyanates or polyisocyanates with polyesters containing hydroxyl groups.

5. A method as claimed in claim 1, wherein the polymer is deposited on the material from a non-polar solvent.

6. A method as claimed in claim 1, wherein the solvent is selected from the group consisting of paraffinic and aromatic hydrocarbons and chlorinated derivatives thereof.

Claims

2. A method as claimed in claim 1 wherein the polymer impregnated material is permanently set by exposing the material to steam at a temperature of at least 100*C for up to 2 hours.
3. A method as claimed in claim 1 wherein the polymer is deposited on the material after cohesive setting thereof, and, following deposition of the said polymer, the material is steam pressed for 2 to 15 seconds to reinforce the cohesive set.
4. A method as claimed in claim 1, wherein said reactive polymer is selected from the group consisting of polyurethanes, polyacrylates, polysulphides, polyoxyalkylene resins with attached thiol groups, polyurethanes with blocked isocyanate groups, and mixtures of blocked isocyanates or polyisocyanates with polyesters containing hydroxyl groups.
5. A method as claimed in claim 1, wherein the polymer is deposited on the material from a non-polar solvent.
6. A method as claimed in claim 1, wherein the solvent is selected from the group consisting of paraffinic and aromatic hydrocarbons and chlorinated derivatives thereof.