DK167697B1 - APPLICATION OF A SULPHONATED PHENOL FORMALDEHYDE OR SULPHONATED NAPHTHOL FORMALDEHYDE CONDENSATION PRODUCT TO TREAT A TEXTILE ARTICLE OF POLYAMIDE TO MAKE THE RESISTANT RESPONSIBLE TO UNLAMENTALLY UNUSUALLY RESPONSIBLE - Google Patents

Description

DK 167697 B1 In the textile industry, tests have been carried out on various methods of imparting resistance to unwanted soiling, staining or staining to fibers, textiles, upholstery fabrics and carpets. These methods 5 comprise treating the fibers with fluorine compounds, silicon compounds or acrylic compounds. Furthermore, it is known that resistance to unwanted staining can be imparted to a fiber by applying a dye-resistant agent to an already colored or unstained fiber. Many dye-resistant agents, including sulfonated naphthol or sulfonated phenyl-formaldehyde condensation products which work well on polyamide substrates, are available. However, these condensation products have been found to have the disadvantage of yellowing on a fiber substrate upon exposure to environmental conditions such as the presence of NO 2. This problem is particularly striking for light colored textile articles.

The invention relates to the use of a sulfonated phenol-formaldehyde or sulfonated naphthol-formaldehyde condensation product for treating a polyamide textile article to make it resistant to unwanted staining or staining, the use of which is the application of the condensation product to a textile article. pH value between 1.5 and 2.5 to reduce yellowing of the treated article due to exposure to 'NO2 in the atmosphere.

The invention provides a drastic reduction in the unwanted yellowing of polyamide textile articles containing sulfonated naphthol or sulfonated.

30 phenol-formaldehyde condensation products (hereinafter referred to as "condensation products" or "stain-resistant agents") resulting from exposure of the treated articles to environmental conditions such as the presence of NO2 in the atmosphere.

When these condensation products are applied to colored textile materials, they have the advantage of acting as resistance to subsequent staining or staining by accidental spillage of certain products such as coffee, red wine and soft drinks. The latter products often contain dyes, such as Food Drug & Cosmetic (FD&C) red no.

40. When e.g. a liquid containing FD & C Red No. 40 is spilled onto a polyamide material, colors (i.e., spots) to that material to a significant degree. However, if the material 10 is first treated with a stain resistant agent, the spilled dye does not provide any permanent staining or staining of the carpet as the unwanted color can be washed out.

Dye resistant agents effective in polyamide materials from the class of sulfonated naphthol or sulfonated phenol-formaldehyde condensation products are disclosed in U.S. Patent No. 4,501,591 and in other patent and professional literature. Typical examples of such stain resistant agents are commercially available products such as Erionol% W (Ciba-Geigy), Intratex% (Crompton & Knowles) and Mesitol®NBS (Mobay). These products are sold in the textile trade for use as dye-resistant agents or as agents for improving wet strength in the treatment of textile materials in baths and are recommended for use at an acidic pH range of 'ca. 4-6.

Although polyamide materials which have been treated with the above stain resistant agents have excellent stain and stain resistance, they present a distinct disadvantage in that they turn yellow upon exposure to certain environmental conditions such as NO 27 which are usually present in the atmosphere and are particularly abundant in urban areas. This yellowing may be severe enough to prevent the application of the dye-resistant agents to light tint textile articles, which are the objects where a staining or staining resistance would be most desirable.

3 DK 167697 B1

In the application of the invention, stain resistant agents are applied to polyamide materials so that the yellowing of these materials is minimized. It includes application: of the dye-resistant agent on the polyamide-5 textile material at a pH between 1.5, 2.5 and 2.5 rather than at pH values of 4-6. As shown in Example 5, the textile materials are significantly better protected against subsequent yellowing under the influence of NO 2 in the atmosphere by the application of the stain resistant agents in this way. Furthermore, the application of the stain resistant agents at pH below about 2.5 for greater adsorption of the agents onto the polyamide than occurs in higher pH ranges. Therefore, not only does the yellowing diminish, but there is also the added advantage that the stain resistant agents can be applied in a more efficient and economical way due to the stronger adsorption of the agents at lower pH values.

In a preferred embodiment of the use of the invention, a textile article (e.g., a blanket) is first stained to the desired tone, rinsed and then saturated for a period of 20 (20 minutes) with a solution (liquid ratio 30: 1) containing a sulfonated naphthol or phenol-formaldehyde condensation product (to give a final concentration of 0.3 to 1.0% by weight of the article) where the pH of the solution is 2 and the temperature is 77 ° C. The article is then rinsed and further processed as necessary.

The invention may be used in conjunction with polyamide textile material. These materials include textiles, upholstery fabrics and rugs. In practice, the material is treated with the stain resistant agent in a bath of pH between 1.5 and 2.5. Any acid can be used to lower the pH of the bath, but non-corrosive acids such as sulfamic acid, phosphoric acid or citric acid are preferred. It is further preferred that the textile articles be dyed or pigmented prior to treatment with the dye-resistant agents. The concentration of stain resistant agent in the treatment bath and the treatment temperature is not critical. Outer- 4

DK Ί67697 BT

Equal fiber treatment compounds may be present in the bath.

Experimental methods 5 Color experiments

A liquid solution for staining or staining carpets is prepared by dissolving FD&C Red No. 40 in water at a concentration of 0.1 g / liter. Alternatively, a commercially available beverage powder with cherry flavor 10 and sweetened with sugar containing FD&C Red No. 40 in water is dissolved to give a solution containing 0.1 g / liter FD&C Red No. 40. 30 ml of the color solution is placed in an aluminum pan of 7.6 x 10.2 cm. A polyamide fiber blanket is used in this experiment, but any textile material containing polyamide fibers can be used. A 6.4 x 8.9 cm piece of the rug to be examined is completely immersed with the face (studs) down in the color solution for 1 hour. The blanket sample is then removed from the dye solution, rinsed thoroughly with running water and dried in an oven for 15 20 minutes at 100 ° C. The rug's resistance to staining or; stain is visually judged by the amount of red color given the blanket of the color solution. A rug rated color-resistant has no red color or only a slight trace of color after staining or staining and rinsing. A 25 rug rated non-color resistant has a deep red color after staining and rinsing.

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Yellowing test with NO2

The sample to be tested is exposed to 2 ppm (parts 30 per million) of NO 2 at a relative humidity of --83 ± 5% and a temperature of 40 ± 5 ° C for 24 hours (one cycle) in a gas inlet chamber (model GE-15, Atlas Devices Company, Chicago, Illinois). The color change was measured on a colorimeter Mac-beth®1500 using Illuminant C. After effect of NO2, the sample is compared to an unaffected sample, and the result is stated as Ab-ι- (yellowing), with increasing positive values of b corresponds to increasing values of yellowing. Carpet samples to be examined are placed in a round specimen holder (diameter 22 mm) with the studs facing a glass lid.

A weight of 4.5 kg is placed on the blanket sample in the holder and 5 pushes the studs against the glass lid. The weight is conveniently applied to the sample using an AATCC Perspiration Tester apparatus (see AATCC test Method 15-1979) in combination with a cylindrical piston that fits into the sample holder. The Ab + value of the compressed sample is read through the glass lid of the sample holder.

Adsorption of the stain resistance agent on the fiber.

Depletion of the dye-resistant agent 15 from the treatment bath on the polyamide fiber material is indicated as percent depletion and is determined by measuring the light absorbance of the bath at a wavelength of 293 nm before and after the treatment.

Example 1

A nylon 6.6 yarn of 68 filaments of trilobal cross-section (1140 denier total -1267 dtex) with stretched and bulk continuous filament is prepared by a conventional method. Two of these yarns are used and twisted to give 25 a yarn with a balanced twist of 1.4 rpm. The yarn produced is then heat-fixed in a Superba heat-fixing apparatus (132 ° C). From the heat-fixed yarn, a tufted rug with cut plywood is made with the following specifications: 1250 g / m2, 19mm pile height, 3/16 gauge, 44 stitches / dm. This blanket is stained to a light blue tone using a conventional color bath batching process and color aids (the color composition is as follows, based on the weight of the blanket: 0.0022% CI Acid Yellow 219, 0.0021% CA Acid Red 361, 0.0219% CI Acid Blue 277; pH = 6.0). After staining, the rug is rinsed and then treated in a bath containing the stain resistant liquid Intratex®N. This DK 167697 B1 6 bath is made by diluting the stain resistant agent with water. An amount of liquid Intratex®N equal to 2% of the weight of the blanket to be treated is used and the pH of the bath is set to 2 with sulfamic acid (approx.

0.5-1.0 g / liter). Place the rug in the bath at a liquid ratio of 30: 1 for 20 minutes at 77 ° C and then rinse. The rug is removed from the bath and dried at 121 ° C. The percent depletion of the dye-resistant agent from the bath is measured at 79%. The blanket is tested for resistance to staining or staining by the method described above and is found to be resistant to staining or staining. Yellowing caused by NC> 2 is investigated by the method described above. The Ab + value is 3.39. Omitting the staining resistance treatment results in an Ab + value of 0.85.

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Example 2 (Comparison ^

A blanket is prepared and treated as in Example 1, except that the pH of the treatment bath is set to 5 using an acetic acid / sodium acetate buffer. The 20 percent depletion is set at only 67%. This is a lower depletion ratio than that measured using a bath of pH = 2. The blanket is treated for and found to be resistant to staining or staining. In the NO2 impact test, the blanket turns yellower than that of Example 1, having an Ab + value of 4.05.

Example 3

A blanket is prepared and treated as in Example 1 except that the dye-resistant agent 30 used was Mesitol® NBS powder. Treatment solution is prepared by dissolving the stain resistant agent in water to a concentration of 0.56% of the Mesitol® NBS powder in relation to the weight of the carpet to be treated. The pH of the bath is then adjusted to 2 with sulfamic acid. The percentage of depletion is measured at 72%. The rug is tested for and found to be resistant to staining, and the Ab + value DK 167697 B1 7 is also 2.83.

Example 4 (Comparison)

A blanket is prepared and treated as in Example 3 I

5 except that the pH value of the dye-resistant treatment solution is adjusted to 5 with an acetic acid / sodium acetate buffer. The percentage depletion is found to be only 61%. The rug is treated for and found to be resistant to staining. In the NO2 impact test, the blanket 10 glows more than that of Example 3, having an Ab + value of 4.17.

Example 5

A blanket of the same structure as that of Example 1 is subjected to a dye-like process in which the dyeing process is carried out without the presence of a dye. Six blanket samples are treated with Mesitol®NBS by the same procedure as in Example 1 except that the pH values of the treatment solutions vary in the range of 2-5. The blanket samples are tested for their resistance to yellowing caused by NO2 20 by the method described above, except that the samples are · exposed twice. The results of the NC 1 yellowing experiment are listed in Table I. A significant reduction in the Ab + value is observed when the stain resistant agent is applied at pH 2.5 to pH 3.0.

Table I

pH Ab-f value 2.0 7.30 2.5 7.71 3.0 9.57 30 3.5 10.27 4.0 10.65 5.0 10.67

Claims (3)

Use of a sulfonated pheno 1 - form 1 dehydric or sulfonated naphthol-formaldehyde condensation product for treating a polyamide textile article to render it resistant to unwanted staining or staining, characterized in that the condensation product is applied to the textile article at a pH. value between 1.5 and 2.5 to reduce yellowing of the treated article due to exposure to NO2 in the atmosphere. Use according to claim 1, characterized in that the textile article is dyed or pigmented before the application of the condensation product. Use according to claim 1, characterized in that the textile article is a colored polyamide fiber blanket. 15