JPH02264071A - Prevention of staining - Google Patents

Abstract

PURPOSE: To obtain stain resistance rich in durable wet fastness by simultaneously or sequentially treating polyamide or keratinous fibers or their product with a fluorocarbon composition, a stain-blocking agent, and a wet color fastness- improving agent in an aqueous bath at a large bath ratio. CONSTITUTION: Polyamide or keratinous fibers, especially wool fibers or their product, especially a domestic wool product, is treated with a fluorocarbon composition in a bath ratio of 1:10 to 1:10O in an aqueous bath under an acidic condition of pH 2-5, preferably pH 3 using sulfamic acid, treated with a stain- blocking agent, and further pre-treated or post-treated with an inorganic salt in order to improve the wet fastness of the stain-blocking effect and its durability, or simultaneously treated with both the stain-blocking agent and the fluorocarbon composition, thereby improving the durability of the wet fastness.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for treating fiber materials and articles, and in particular to a method for treating fibers and articles to improve stain resistance.

Household upholstery textiles, especially carpets, are subject to contamination during use, and it is often inconvenient to subject them to washing operations. For example, nylon carpets are coated with stain inhibitors (5 stain-b) to increase their resistance to staining.
fluorocarbons) and/or with compounds known as fluorocarbons. One commonly used method that is compatible with finishing processes not used for nylon carpets is to treat the fibers with a stain inhibitor in a dye bath and subsequently spray fluorocarbons onto the finished carpet. be.

One disadvantage of this method is that contaminating liquids often seep through to the back of the carpet. After the first wash, the immediately affected area on the top of the carpet pile will be cleansed of dirt, but dirt on the backside will tend to be picked up by the pile and stain the area around the original area. be. Application methods used in connection with nylon carpets may not be applicable to household furnishings made from other fibers, such as keratinous fibers such as wool. Another drawback associated with many existing treatments is their limited fastness to shampooing and abrasion.

The object of the invention is a method of applying stain inhibitors and fluorocarbons to keratinous and polyamide fibers.

It will become clear from the following description that the invention is given by way of example.

According to the broadest aspect of the present invention, there is provided a method for improving the stain resistance of polyamide and keratin fibers and textiles, which method comprises producing melon fibers and textiles at a long liquor ratio in an aqueous dyebath. , first with a fluorocarbonate composition and then with a stain inhibitor.

The present invention further provides a method for improving the durability and wet fastness of the stain protection effect produced.

The joint use of an antifouling agent and a fluorocarbon has been found by the inventors to be a preferred measure, since the antifouling agent increases resistance to staining (with liquid colorants), but it actually can have deleterious effects when contaminated, and the use of an effective repellent/anti-stain finish, such as that provided by fluorocarpanes, is essential to the overall effect, both of which reduce its resistance to contamination. This is because it improves the fiber's resistance to staining without reducing its resistance.

Since the fluorocarbon imparts a polymeric coating to the fibers, it is believed that it should be applied subsequent to the antifouling agent, or at least simultaneously so as not to interfere with the absorption of the latter. Surprisingly, it has been found in accordance with the present invention that very good results are obtained by first applying the fluorocarbon and allowing it to exhaust the fibers in the same bath before applying the stain inhibitor.

The inventors have found that simultaneous application results in interference between the fluorocarbon and antifoulant, incomplete exhaustion, and therefore inferior results. Also, application of the fluorocarbon following the antifouling agent in the same bath does not give as good results as the process of the present invention.

Although the effectiveness of the present invention is not bound by any theory, it is believed that the antifouling agent is not completely exhausted and that residual antifouling agent in the bath interferes with the application of the fluorocarbon. When using a fresh bath for fluorocarbon application, it is believed that antifouling agents on the fiber surface interfere with fluorocarbon application.

The process of the invention is particularly advantageous for wool fibers and textiles, especially wool furnishings. This method can be applied at the loose wool, roving, slubbing, yarn or finished fiber article stage. Advantageously, the method is applied in a dyebath immediately following the dyeing or bleaching of the fibers.

The vine stain inhibitors used in the process of the invention are those commonly available for this purpose, such as those described in European Patent Publication No. 0242.
There are those described in No. 495 and No. 0242496. Such compounds are available on the market, among others under the trade names Granofin WG (Granofin WG), Mesitol NBS (Mesit).
ol NBS: Byz A/), Algard WR (
Alguard WR Nearride Colloid), Er1onal RF (Cibar Geigy), or Scotchguard FX 369 (Scotch
guard FX 369: 3M Corporation), typical examples include sulfonated phenol-formaldehyde or naphthol-formaldehyde condensation products, in which the product is a sulfonic acid bonded to the carbon atom of the phenol or nalatol group. A preferred product containing the group (-SO,H) or a salt thereof (e.g. an alkali metal salt) is typically a condensation product of phenolsulfonic acid or narlatolsulfonic acid and bishydrocyphenylsulfone. I can do it. Furthermore, compounds commercially available as synthetic tanning agents, such as Baykanol HLX (Baykanol H
LX: Peyer) and Tanigan OS (Tanigan OS)
OS: Peyer) was also found to be effective.

Fluorocarbons useful in the process of the invention should be characterized in that they should have good soil repellency properties and be compatible with subsequent application conditions, such as those that do not become de-exhaustive under low pH conditions. You can choose from those commonly used for processing five items.

A preferred fluorocarbon has the trade name Teflon TO (Tef
lon TC: Dubon), Scotchgard FC397
(Scotehguard FC397: 3M)
, Scotchgard F0396 (3M), and Scotchgard FX3602 (3M). Representatives include acrylate or urethane backbones with pendant fluorinated alkyl groups.

The process is advantageously carried out under acidic conditions, typically 1) H2-5, especially pH 3; the pH can be adjusted with sulfamic acid. The temperature is preferably elevated and can range from 30 to 100<0>C, especially from 50 to 80<0>C.

This method is an exhaustion method from longer wavelength, and l:10-1
A liquid:workpiece ratio of :100 can be used, typically 1:30.

It has been found that the results of the method of the invention can be enhanced by carrying out other methods in addition.

First, it has been found that pre-treatment or preferably post-treatment with inorganic salts for stain inhibitors improves the performance of treated fibers in terms of abrasion resistance and wet fastness. Although the addition of different electrolytes would be expected to retard exhaustion (at low pH), we surprisingly found that certain zirconium and IWlium salts have an advantageous effect compared to other electrolytes. was discovered. Not only is stain resistance improved, but abrasion resistance and wet fastness of the process are also enhanced.

Various auxiliaries can be added to the dyebath to facilitate exhaustion and/or dispersion of the stain inhibitor.

The effects generally seen were merely redundant. However, two special adjuvants used for low-temperature dyeing of sheep, Baylan NT (Beylan NT)
and Lanasin LT (Sandoz)
gave a very significant improvement to this method.

Carpets are often treated with steam during normal finishing operations. However, it has surprisingly been found that atmospheric steam treatment of carpets treated according to the method of the invention substantially improves the anti-fouling effect. It is therefore preferred to post-treat the carpet treated according to the method of the invention with steam, for example for 1 to 5 minutes, especially for about 2 minutes.

Particularly preferred carpet treatment steps are: Start at 20°C with a long wave of 1:20 to 1:60.

Add 2% fluorochemical (sulfamic acid) at pH 3.

The temperature is increased to 50°C at a rate of 1°C/min and treated at 50°C for 30 minutes.

Add 8% antifouling agent and 2% adjuvant.

Readjust the pH to 3-3.5 (sulfamic acid).

Raise to 65°C at 1°C/min and treat at 65°C for 30 minutes.

9 baths available. Wash with water and dry.

The processing sequence described above is carried out in a bath, preferably in a dyebath following the dyeing operation.

The following fixing treatments can be used as pre- or post-treatments if desired. For pretreatment: start at 20° C. with a liquid ratio of 1:60.

Add fixation chemicals, low smoke Zirpro formulation (containing zirconium acetate) or Aj, (So, ), .16H,O.

Increase to 70°C at 1°C/min. Treat for 30 minutes and continue with the preferred processing steps described above.

For post-treatment = 30 minutes at 65°C, then the fixing chemicals are added. After 15 minutes, remove from the bath and wash with cold water.

Wash with water and dry.

After manufacture, the carpet pile should preferably be manually steamed for two minutes.

If the carpet is of tuft or cut pile construction,
The finished carpet is then oversprayed with a fluorocarbon or stain inhibitor/fluorocarbon mixture;
It may be desirable to seal the cut edges to increase resistance to contamination and improve the durability of anti-contamination treatments.

Carpets treated with some type of carpet treatment, such as the Ronz Chemist process, have sufficient setting to allow piece dyeing without significant loss of tuft shape. Since the method of the invention is applied after dyeing, the carpet is treated in an exhaust solution without the need to overspray the carpet.

The invention is further illustrated by examples.

Evaluation Methods Evaluation of Resistance to Abrasion Fabric samples were rubbed against a standard abrasion fabric using a Martinzol abrasion tester with 500 rubs. The sample was then contaminated.

Evaluation of wet fastness Detergent solution (anionic detergent 10d/7, p) I7.5
．． 40°C) was applied under pressure and removed under reduced pressure using a spray extractor. This cleaning method was repeated five times by the woodcutter. The dried samples were then contaminated.

Contamination Method Fabric treatment was carried out using a contamination solution (0,811/l FD+C Red 4
0.411/l citric acid, o, 1 g/) nonionic wetting agent). Excess solution was gently shaken off. The samples were left uncovered on a polyethylene sheet for 24 hours at room temperature, washed with cold water until no more dirt was removed, and dried for 30 minutes at 30-70°C.

Measurement of contaminated wool The color difference compared to the untreated sample was measured using ICS Micromatch (
It was measured as ΔE (CMC) using Micromitch).

Contamination prevention treatment for wool Treatment E (24 hour contamination) Untreated 110% SR, steam treated 30.2 32.2 36.3 7.9 11,3 32.9 FC = Sulfocarbon (Scotchgard FC397)
. SB = anti-fouling agent (Megitol NBS).

Contamination prevention treatment for nylon 6 and 66 Treatment E (24 hours) Example Nylon 6 Nylon 66 untreated 52.7 43.37 5%
Meditol NBS 3.9 3
．． 3 All fluorocarbon and antifoulant treatments are
pH 3-3 adjusted with sulfamic acid at 65 °C for 0 min.
, 5 was applied. All concentrations are based on wool weight.
Shown as supplied.

Some test results on carpets are shown in the drawings,
Figure 1 shows a durability test using a Hexabod fist carpet abrasion tester. For the carpet sample, a solution of food dye amaranth 0.089/1 was used, and 10 m of the dye solution was
The staining was introduced onto the carpet surface using a standard staining device that uniformly applied the dye solution over a circular area of 80 IIK diameter. This was left to dry for 24 hours and decontamination was planned using a commercially available hot water extraction carpet washer using an appropriate detergent. The carpet was then allowed to dry and the residual stain density was measured using a Minolta Chromameter CR110, and the results were calculated as a color difference (ΔE) relative to the unstained carpet.

From Figure 1, Baykanol HLX (Baykanol
HLX) The treated carpet has a good initial resistance to staining (8E2), but after the carpet has undergone abrasion in the aging pot, it remains better than the untreated carpet, but the resistance to staining remains better than the untreated carpet. It can be seen that the speed has decreased (ΔE of 25 after 1000 rotations).

However, the carpets treated with Baikanol HLX, Pylan NT and with aluminum sulfate after treatment show very good resistance to post-abrasion staining (ΔE5 after iooo revolutions).

FIG. 2 shows the staining results after various shampoo treatment cycles. The Pykanol HLX treated sample showed a slight decrease in stain resistance after shampooing, while the Pylan NT and aluminum sulfate post-treatments as adjuvants showed virtually no decrease in stain resistance after shampooing.

Accordingly, the present invention provides a method for preventing contamination of textile materials and articles.

Although particular embodiments of the invention have been shown, it will be obvious that modifications may be made thereto without departing from the scope of the claims.

[Brief explanation of drawings]

FIG. 1 is a diagram showing the results of the durability test of the abrasion test, and FIG. 2 is a diagram showing the staining results (fastness) after the shampoo treatment cycle. Procedural amendment (θ Procedural amendment C format) % formula % )) Moat Pme fills in 3゜ Person making the amendment 3゜ Person making the amendment = Relationship with lf matter Punch λ′f Entered person 4゜Agent pI-//1. - Folding pill 6th floor (・u story'<2F 5゜Date of amendment order November 13, 1999 (shipment mortar 28) November 1999 6゜Column of patent applicant of application subject to amendment Power of Attorney Corporate and Nationality Certificate Drawing 7゜Contents of amendments are as attached, and the drawings are engravings). (Please change the contents 8゜ Attached document list 1) Request i! (Accurately stating the address of the patent applicant and the name of the representative) 2) Power of attorney and its translation (2 copies each) 4) Drawing (engraved) 1 copy

Claims (1)

[Claims] 1. Polyamide and keratin fibers and textile products, characterized in that the fibers or textile products are treated first with a fluorocarbon composition at a long liquor ratio in an aqueous dyebath and subsequently with a stain inhibitor. A method of improving the stain resistance of. 2. The method of claim 1 further comprising a treatment to improve the wet fastness and durability of the stain control effect produced. 3. The method of claim 2, wherein the wet fastness and durability are improved by the simultaneous use of a stain inhibitor and a fluorocarbon. 4. The method of claim 3, wherein the fluorocarbon is first applied and the fiber is exhausted before applying the stain inhibitor in the same bath. 5. A method according to any one of claims 1 to 4, wherein the fibers and textile products are woolen fibers and textiles, in particular woolen household textiles. 6. A method according to claim 5, wherein the method is applied at the step of producing loose wool, lobing, slubbing, yarn or textiles. 7. A method according to claim 6, wherein the method is applied in a dye bath immediately following the dyeing or bleaching of the fibers. 8. The antifouling agent used is European Patent Publication No. 024.
No. 2495 and No. 0242496 and commercially available compounds, especially under the trade name Granofin WG.
(Hoechst A.G.), Meditor NBS (Payer), Algard WR (Allied Colloid), Elional RF (Ciba, Geigy), or Scotch Guard F
8. The method according to any one of claims 1 to 7, wherein the compound is commercially available as X369 (3M Corporation). 9. Baykanor HLX (Payer) and Tanigan OS
9. A method according to claim 8, wherein a synthetic tanning agent such as (Peyer) is used as an antistaining agent. 10. A suitable fluorocarbon has the trade name Teflon TC.
(Dubon) Scotch Guard FC397 (3M)
10. The method according to any one of claims 1 to 9, which is commercially available as Scotchguard FG396 (3M), Scotchguard FX3602 (3M). 11. A process according to any of claims 1 to 10, wherein the process is carried out under acidic conditions, typically at a pH of 2 to 5, in particular at about pH 3. 12. The method according to claim 11, wherein the pH is adjusted with sulfamic acid. 13. Increase the temperature, 30-100℃, especially 50-8
The method according to any one of claims 1 to 12, wherein the temperature is in the range of 0°C. 14. The method is exhaustion method from long liquid ratio, 1:10-1
14. A method according to any of claims 1 to 13, wherein a liquid to workpiece ratio of 1:100 is used, typically a ratio of 1:30. 15. A process according to any of claims 1 to 14, in which a pre- or post-treatment with an inorganic salt is applied with respect to the stain inhibitor to improve the performance of the treated fibers in terms of abrasion resistance and wet fastness.