GB2082215A - Textile finishing - Google Patents

Textile finishing Download PDF

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Publication number
GB2082215A
GB2082215A GB8025357A GB8025357A GB2082215A GB 2082215 A GB2082215 A GB 2082215A GB 8025357 A GB8025357 A GB 8025357A GB 8025357 A GB8025357 A GB 8025357A GB 2082215 A GB2082215 A GB 2082215A
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Prior art keywords
polysiloxane
emulsion
employed
treatment
article
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GB8025357A
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Wool Development International Ltd
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Wool Development International Ltd
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Priority to GB8025357A priority Critical patent/GB2082215A/en
Publication of GB2082215A publication Critical patent/GB2082215A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6436Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

A method of finishing keratinous textiles, especially wool fabrics comprises treating the article with a methyl hydrogen polysiloxane and the reaction product of an epoxide resin with a di and/or polyamine. The articles so treated exhibit water repellent and shrink resistant properties from a single application. Preferably the articles are pre-treated by scouring under alkali conditions with an anionic surfactant, followed by rinsing, to remove surface active agents and ensure that the fabric pH is on the alkali side of neutral.

Description

SPECIFICATION Textile finishing This invention relates to a method of finishing keratinous textiles, and in particular relates to a method of applying a water repellent and shrink resistant finish thereto.
The natural water repellency of wool textiles is high but for special end-uses, for example, protective clothing where resistance to penetration of splashes of obnoxious or corrosive chemicals is desirable, additional treatments to enhance water repellency of the textile articles may be required.
Protective clothing for use in industry is subject to soiling and for reasons of simplicity and economy is generally laundered in order to cleanse it. As is well-known, untreated wool textiles intend to shrink when laundered and so it would be desirable if a combined water repellent and shrink resistant finish could be applied to wool textile articles.
Attempts to combine a water repellency treatment with one of the currently available shrink resistant finishes for wool textile articles have not met with a great deal of success. To start with most shrink resist finishes involve the use of anionic agents and, since most of the water repellent agents are cationic, the components tend to interact unfavourably. Furthermore most of the shrink resist systems require different curing conditions than those required by the water repellent agents; and even where satisfactory shrink-resistance was obtained it has been found that water repellency is adversely effected.
The present invention seeks to provide a method of imparting a water repellent and shrink resistant finish to keratinous textile articles using a single system.
According to the present invention there is provided a method finishing keratinous textile articles which comprises treating the articles with a methyl hydrogen polysiloxane and the reaction product of an epoxide resin with a di- and/or polyamine.
The methyl hydrogen polysiloxane is preferably end blocked, for example with trimethyl siloxyl end groups. Such compounds have viscosities of 10-25,000 c.st, typically about 1 5 c.st. The polysiloxane may be used either on its own or together with a silicone oil, that is dimethyl polysiloxane, methylphenyl siloxanes, or diphenyl siloxanes, again end blocked with, for example, trimethyl siloxyl groups, or combinations of methylphenyl or diphenyl groups. Such compounds have viscosities in the range 1 0-2,500,000 c.st; at 200 C, typically about 15,000 c.st. Conveniently the polysiloxanes are in the form of aqueous emulsions, and other component such as emulsifying agents and organic solvents may also be present in the emulsions.
The reaction products may be prepared by various methods, and preferred products are those obtained when epoxide resins, such as the reaction product of one mole of 4,4'-di-p-hydroxyphenyi- 2,2'-propane and two moles epichlorhydrin are reacted with di- and/or polyamines containing at least two reactive hydrogen atoms, such as methylene diamene, tetromethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine, a,a'-diaminopropylmethylamine and piperazine in proportions such that 1 to 3 epoxide groups are employed for each reactive hydrogen atom or the amine.The reaction products may be employed in the form of salts or readily volatile organic acids, such as acetic acid, in aqueous solution, or may be employed as emulsions, especially the latter since such emulsions have a higher pH.
The quantities of agents may vary within wide limits subject to the desired and degree of shrink resistance/water repellency required together with such factors as the type of textile substrate, and so on. In general the polysiloxane will be used in amounts of from 1.5% to 10%, with 1% to 5% (by weight on weight of textile) being preferred. The amount of reaction product required in order to give adequate water repellency is quite small, for example from 5% to 20% by weight of the polysiloxane used.
However, we have found that in order to give adequate shrink resistance, the amount of reaction product used must be considerably greater than the amount necessary for water repellency, for example in the range of 30 to 100% of the amount of polysiloxane used.
The keratinous fibres may be for example mohair, alpaca, vicuna, angora, or especially wool; and the textile article may be in the form of loose stock, slivers, slubbings, rovings, yarns, fabrics, made up garments or carpets, preferably fabrics.
The treatment may be carried out in any suitable manner e.g. exhaustion, dipping, spraying or padding, preferably the latter.
In the preferred application by padding, e.g. by using a padding mangle, it has been found that, in order to obtain the necessary wetting out of the fabric being treated, it is preferably to use a wetting agent in the treating liquor. Alcohols are generally recommended as wetting agents for water repellent treatments and we have found that Invadine 3817 (Ciba-Geigy), which is a mixture of alcohols, to be particularly suitable.
It has been found that pH control is important in the practice of the invention. The pH of treatment should be on the alkaline side of neutral. The neutral pH of the reaction products will generally ensure this, but is very important that the plain pH also be neutral to alkaline before treatment.
Since many wool fabrics may have been subjected to acid treatments, such as carbonisation or dyeing, it is necessary to prepare the fabric to ensure that it has the correct pH range. Since it is also necessary to ensure that the fabric is free of surface active agents which may interfere with the water repellency effect, these steps may continually be carried out together in an alkaline scouring step. The fibres to be treated are ideally scoured with an anionic surfactant in the presence of an alkali such as sodium bicarbonate. The use of an anionic surfactant, unusual with keratinous fibres, is preferred since, especially under alkaline conditions, it has little affinity for the fibres and can therefore easily be removed by subsequent rinsing leaving the fibres clean and free from surfactants of any kind.The presence of the alkali ensures that fabrics will now have a pH in the range of 7 to 10.
Although if it is known that a particular fabric is chosen, free from surfactants, and has an alkali pH, it is not necessary to pretreat as described above; as a practical matter it is desirable always to perform the alkali prescour to ensure correct fabric preparation for a treatment of the invention.
If desired co-catalysts known for silicone systems, such as metal salts, may also be employed in the treatment of the invention.
Furthermore, it is possible to allow the reaction products to be formed in situ by applying the silicone together with the epoxide resin and the di- or polyamine (or a precursor thereof) directly to the fibres, either from a solvent or an emulsion, and curing as before.
In the following examples, which are for the purpose of illustration, the various tests described were as follows:- Spray Rating Test Aspray rating test was carried out in accordance with British Standard 3702; 1 964 in which a subjective spray rating on a scale of 1 to 5 is used to represent the water repellent effect. The higher the rating the better the water repellency. The percentage weight increase of the textile material during the test was also determined.
Effect of Washing on Water Repellency The spray rating was also evaluated after 10, 20, 30, 40 and 50 washes at 400C, in accordance with AATCC test method 124-1 975, washing procedure 6.2(1), with a Kenmore washing machine, model 21900, and a commercial detergent (Bold) using 90 grams of detergent per 65 liters of liquor.
The total load was 1.8 kg of samples together with polyester makeweights, and the liquor to goods ratio was 36 to 1. The samples were not dried between washes.
Felting Shrinkage The felting shrinkage of the keratinous textile article was determined in accordance with IWS test method 1 85. In this, one kg of samples (including where applicable polyester makeweights) are washed in 1 5 liters of phosphate buffer solution at pH7 and 400C in a 50-litre International Cubex felting machine. Percentage area of shrinkage is tested after 1 hour and 3 hours of washing.
Examples In the Examples below "emulsion 1 04" is Rhodorsil emulsion 104 (Rhone-Poulenc) which is a 40% solids non-ionic emulsion of a methylhydrogen polysiloxane and a trimethyl siloxyl end blocked dimethylpolysiloxane; "emulsion 4089" is Rhodorsil emulsion 4089 (Rhone-Poulenc) a 30% solids cationic emulsion of polymethylhydrogensiloxane; and "emulsion 6014 is Rhodorsil emulsion 6014 (Rhone-Poulenc), a 20% solids non-ionic emulsion of a reaction product of an epoxy resin and a di and/or polyamine. All percentages are expressed by weight (of solids) based on the weight of the fabric unless otherwise stated.
The fabric treated is a dyed wool gaberdine fabric, 270 gm/m2 (2x2 twill). The fabric is prepared by scouring for 20 minutes at 400C at a liquor ratio of 1:20 in a solution of 5% NaHCO3 o.w.f. and 0.5 g/l of Lerapon C.A. (Bayer), an anionic surfactant, followed by two cold rinses and drying. This ensures that the fabric is clean and at a pH in the range 7 to 10. The fabric is treated by padding on the agents to 7080% wet pick-up, and is then dried before airing for 5 minutes at 1 400C.
The results of the Examples 1 to 12 as shown in Tabies 1 to 3 show clearly that the useful combined water repellency and shrink resistance finish can be applied to wool textile articles from one application using a single system, and this finish is durable to repeated washing.
TABLE 1 DOSAGE OF EMULSION 104 AND EMULSION 6014
Cubex % Felting Water-Repellency Shrinkage After: Initial A10W A20W A30W A40W Examples Treatment 1 hr 3 hr S.R. W.I. S.R. W.I. S.R. W.I. S.R. W.I. S.R. W.I.
1 2% Emulsion 104 + 0.8% Emulsion 6014 0 2 4 1.11 4 0.74 4 2.88 3 3.87 4 4.9 2 3% Emulsion 104 + 0.9% Emulsion 6014 -1 2 3 0.93 4 0.87 4 1.89 5 0.26 4 4.2 3 3% Emulsion 104 + 1.2% Emulsion 6014 0 2 3 1.11 4 0.87 4 1.38 4 1.54 4 4.5 4 4% Emulsion 104 + 1.2% Emulsion 6014 0 0 3 1.71 4 0.82 4 1.18 4 4.09 4 3.8 5 4% Emulsion 104 + 1.6% Emulsion 6014 0 1 3 1.14 4 1.00 4 1.35 4 1.53 4 2.8 6 5% Emulsion 104 + 1.5% Emulsion 6014 -1 -1 4 1.32 4 0.93 4 1.21 4 1.36 4 3.2 7 5% Emulsion 104 + 2.0% Emulsion 6014 -3 -2 4 1.68 4 1.09 4 1.05 4 1.62 4 2.5 Untreated 4 20 3 19.3 - - - - - - - S.R. - Spray Rating W.I. % Weight Increase A10W, A20W, A30W, A40W - After 10 (20) (30) (40) Washes at 40 C (Kenmore) TABLE II DOSAGE OF EMULSION 4089 AND EMULSION 6014
Cubex % Felting Water-Repellency Shrinkage After: Initial A10W A20W A30W A40W Examples Treatment 1 hr 3 hr S.R. W.I. S.R. W.I. S.R. W.I. S.R. W.I. S.R. W.I.
8 4% Emulsion 4089 + 1.2% Emulsion 6014 -2 2 4 1.38 4 1.14 3 4.13 3 9.58 3 14.6 9 4% Emulsion 4089 + 1.6% Emulsion 6014 -1 2 4 1.47 4 1.25 3 3.48 3 6.21 3 9.8 10 5% Emulsion 4089 + 1.5% Emulsion 6014 -2 1 4 0.90 4 0.89 4 #.87 3 4.22 3 8.3 11 5% Emulsion 4089 + 2.0% Emulsion 6014 -2 0 4 1.15 4 1.21 4 2.65 3 7.97 3 10.8 Untreated 4 20 3 19.3 - - - - - - - S.R. Spray Rating W.I. % Weight Increase A10W, A20W, A30W, A40W - After 10 (20) (30) (40) Washes at 40 C (Kenmore) TABLE III
% Area Felting Shrinkage Initial A 10W A20W A30W A40W A50W Cubex Examples Treatment SR % Wl SR % Wl SR % Wl SR % Wl SR % Wl SR % Wl 1 hr 3 hr A 10W A20W A30W A40W A50W 13 4% Emulsion 5 0.8 4 1.3 4 2.61 4 2.91 4 0.9 4 1.4 -1 2 0% 2% 2% 2% 2% 104 o.w.f.
1.6% Emulsion 6014 o.w.f.
+ 15 g/l In vadien 3817 5 1.1 4 2.1 4 3.4 4 4.1 4 1.5 4 1.5 10 m of Orange Gaberdine treated in the Pilot Plant Fabric was padded once through the pad mangle-tenter dried 140 C - Cured 1 m/minute at 140 C.
A10W, A20W, A30W, A40W, A 50W - After 10, 20, 30, 40, 50 washings at 40 C in the Kenmore Washing Machine.
S.R. - Spray Rating % WI.I. - % Weight Increase.

Claims (28)

1. A method of finishing keratinous textile articles which comprises treating the articles with a methylhydrogenpolysiloxane and the reaction product of an epoxide resin with a di and/or polyamine.
2. A method as claimed in claim 1 in which the methylhydrogenpolysiloxane is end blocked with trimethylsiloxile end groups.
3. A method as claimed in either of claims 1 or 2 in which the methylhydrogenpolysiloxane has a viscosity in the range of 10 to 25,000 c.st.
4. A method as claimed in claim 3 in which the viscosity is about 1 5 c.st.
5. A method as claimed in any one of claims 1 to 4 in which silicone oil is used together with the polysiloxane.
6. A method as claimed in claim 5 in which the silicone oil is a dimethylpolysiloxane, a methylphenyl siloxane, or a diphenylsiloxane, end blocked with trimethylsiloxile groups, or combinations of methyl, phenyl or diphenyl groups.
7. A method as claimed in claim 6 in which the silicone oils have viscosities in the range 10 to 2,500,000 c.st.
8. A method as claimed in claim 7 in which the viscosity is about 15,000 c.st.
9. A method as claimed in any one of claims 1 to 8 in which the polysiloxanes are in the form of aqueous emulsions.
10. A method as claimed in any one of claims 1 to 9 in which the reaction product is formed from the product of a reaction of one mole of 4,4'-di-p-hydroxyphenyl-2,21-propane and two moles epichlorhydrin.
11. A method as claimed in any one of claims 1 to 10 in which the di and/or polyamine is selected from ethylenediamine, tetramethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine, ,ct'-diaminopropyímethyíamine and piperazine.
12. A method as claimed in any one of claims 1 to 11 in which the oxide and di or polyamine are employed in proportions such that there are 1 to 3 epoxide groups for each reactive hydrogen atom of the amine.
1 3. A method as claimed in any one of claims 1 to 12 in which the polysiloxane is used in an amount of from 0.5 to 10% by weight on the weight of the textile article.
14. A method as claimed in claim 13 in which the polysiloxane is employed in an amount of 1 to 5%.
1 5. A method as claimed in any one of claims 1 to 14 in which the amount of reaction product employed is in the range of 13 to 100% by weight of the amount of polysiloxane employed.
1 6. A method as claimed in any one of claims 1 to 1 5 in which the keratinous fibres are selected from mohair, alpaca, vicuna, angora, or sheeps wool.
17. A method as claimed in any one of claims 1 to 1 6 in which the textile article may be in the form of loose stock, silvers, slubbings, rovings, yarns, fabrics, made up garments or carpets.
1 8. A method as claimed in claim 1 7 in which the textile article is in the form of a fabric.
19. A method as claimed in any one of claims 1 to 1 9 in which the treatment is carried out by exhaustion, dipping, spraying or padding.
20. A method as claimed in claim 1 9 in which the treatment is carried out by padding.
21. A method as claimed in claim 20 in which a wetting agent is employed in the treatment of liquor.
22. A method as claimed in claim 21 in which the wetting agent is an alcohol.
23. A method as claimed in any one of claims 1 to 22 in which the textile article is subjected to an alkali scour before treatment with the polysiloxane and reaction product.
24. A method as claimed in claim 23 in which the scouring agent is an anionic surfactant.
25. A method as claimed in either of claims 23 or 24 in which the article is thoroughly rinsed after scouring.
26. A method as'claimed in any one of claims 1 to 25 in which the article to be treated and the treatment liquor has a pH above 7.
27. A method of finishing keratinous textile articles substantially as hereinbefore described with reference to and as illustrated in the foregoing examples.
28. A keratinous textile article whenever treated by a method as claimed in any one of claims 1 to 27.
GB8025357A 1980-08-04 1980-08-04 Textile finishing Withdrawn GB2082215A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0315477A2 (en) * 1987-11-05 1989-05-10 Precision Processes Textiles Method for the treatment of wool
FR2649732A1 (en) * 1989-07-13 1991-01-18 Kanebo Ltd WASHABLE SILK ETOFFE AND METHOD FOR PREPARING THE SAME
US5445652A (en) * 1988-12-06 1995-08-29 Precision Processes Textiles Method for the treatment of cellulosic fibres with amino functional and silicone polymers
US5837370A (en) * 1995-06-30 1998-11-17 E.I. Du Pont De Nemours And Company Fabrics of wool and/or polyester fibers
EP1076078A1 (en) * 1999-08-07 2001-02-14 Ciba Spezialitätenchemie Pfersee GmbH Polysiloxane compositions for wool treatment
US6783806B2 (en) 2000-04-04 2004-08-31 Ciba Specialty Chemicals Corporation Silicone compositions for treating wool materials
US6803407B2 (en) 2000-03-16 2004-10-12 Ciba Specialty Chemicals Corporation Polyorganosiloxanes having alkoxylated side chains
CN106835710A (en) * 2017-01-17 2017-06-13 常熟市新光毛条处理有限公司 A kind of Australia's wool top complete easy-care finishing technique

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0315477A2 (en) * 1987-11-05 1989-05-10 Precision Processes Textiles Method for the treatment of wool
EP0315477A3 (en) * 1987-11-05 1990-01-17 Precision Processes (Textiles) Limited Method for the treatment of wool
US5087266A (en) * 1987-11-05 1992-02-11 Precision Processes (Textiles) Limited Method for the treatment of wool
US5445652A (en) * 1988-12-06 1995-08-29 Precision Processes Textiles Method for the treatment of cellulosic fibres with amino functional and silicone polymers
FR2649732A1 (en) * 1989-07-13 1991-01-18 Kanebo Ltd WASHABLE SILK ETOFFE AND METHOD FOR PREPARING THE SAME
US5837370A (en) * 1995-06-30 1998-11-17 E.I. Du Pont De Nemours And Company Fabrics of wool and/or polyester fibers
EP1076078A1 (en) * 1999-08-07 2001-02-14 Ciba Spezialitätenchemie Pfersee GmbH Polysiloxane compositions for wool treatment
US6579325B1 (en) 1999-08-07 2003-06-17 Ciba Specialty Chemicals Corporation Silicone compositions for treating wool materials
US6803407B2 (en) 2000-03-16 2004-10-12 Ciba Specialty Chemicals Corporation Polyorganosiloxanes having alkoxylated side chains
US6783806B2 (en) 2000-04-04 2004-08-31 Ciba Specialty Chemicals Corporation Silicone compositions for treating wool materials
CN106835710A (en) * 2017-01-17 2017-06-13 常熟市新光毛条处理有限公司 A kind of Australia's wool top complete easy-care finishing technique

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