JPS63552B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a polyester synthetic fiber fabric that prevents graying during dry cleaning, easily removes stains during water-based washing, and is resistant to re-staining, and a method for producing the fabric. When polyester-based synthetic fiber products are dry-cleaned, there are many accidents in which white and light-colored items turn dark, but this phenomenon is caused by dirt accumulated in the dry cleaning bath back-contaminating the polyester-based synthetic fibers. It is thought that this happens because of the Since dry cleaning baths are solvent-based, their ability to suspend dirt is lower than that of water-based washing baths. Therefore, dirt that falls off from textile products becomes fine particles and disperses in the solvent, but this is the main reason for polyester synthesis. It is redeposited onto the fibers, causing a graying phenomenon. Once graying stains adhere, they are extremely difficult to remove and return to their original state. In order to avoid this graying phenomenon during dry cleaning, the dry cleaning industry is currently taking precautions such as cleaning lightly colored items with little dirt and items with heavy dirt in separate baths. However, there are cases where accidents occur during dry cleaning, resulting in complaints regarding polyester synthetic fiber products. For white items and very light-colored textile products, stains are noticeable on the edges and cuffs that come into contact with the skin, and these stains are difficult to remove with simple washing with water, and repeated washing can cause the stains to re-adhere and darken. This is often seen as a graying phenomenon. The present invention was made in view of the current situation, and
The purpose of this invention is to process a polyester synthetic fiber fabric that will not cause graying during water-based or solvent-based washing.
In order to achieve this object, the present invention has the following configuration. That is, the present invention provides polyester synthetic fiber fabric with dimethylpolysiloxane having an average degree of polymerization of 30 to 500 and having a hydroxyl group directly bonded to silicon at the terminal, or methylhydrodienepolysiloxane having an average degree of polymerization of 10 to 80, alone or in a mixture of both. 0.05% or more of polysiloxane resin based on the weight of the fiber, 0.05% or more of alkyl etherified methylol melamine resin based on the weight of the fiber, and an average molecular weight of
A polycondensate of polyethylene glycol of 500 to 3,000 and terephthalic acid with an average degree of polycondensation of 3 to 10 is attached to the fiber in an amount of 0.1% or more based on the weight of the fiber, and then
A method for producing a polyester synthetic fiber fabric having graying prevention properties in water-based and solvent-based washing, characterized by heat treatment at 200°C, and the constituent fibers of the fabric have a hydroxyl group directly bonded to silicon at the terminal end. Polycondensation of polysiloxane resin consisting of one or both of dimethylpolysiloxane and methylhydrodiene polysiloxane at 0.05% or more based on the fiber weight, alkyl etherified methylolmelamine resin at 0.05% or more based on the fiber weight, and polyethylene glycol and terephthalic acid. This is a polyester-based synthetic fiber fabric having anti-graying properties, characterized in that it contains 0.1% or more of a compound based on the weight of the fibers. The fabric of the present invention is a resin obtained by polycondensation of a polysiloxane resin made of dimethylpolysiloxane or methylhydrodiene polysiloxane alone or a mixture having a hydroxyl group directly bonded to silicon at the terminal, an alkyl etherified methylolmelamine resin, and polyethylene glycol and terephthalic acid. It is obtained by applying a mixed emulsion consisting of the following, followed by drying and heat treatment, thereby imparting graying prevention properties to polyester synthetic fiber fabrics in water-based and solvent-based washing. The present invention will be explained in detail below. In order to clarify the correlation between the graying phenomenon in water-based and solvent-based washing and fiber processing agents, the present inventors conducted repeated experiments with a number of textile processing agents, and found that the graying phenomenon in water-based washing was The inventors have discovered that a polycondensate of polyethylene glycol and terephthalic acid is effective in preventing graying, and the polysiloxane resin and As a result of further research on combining melamine resins, we have found that the three components of a special polyethylene glycol and terephthalic acid polycondensate, polysiloxane resin, and melamine resin can be used as a mixed emulsion, or some of the components can be placed in a separate bath. The present invention provides two-stage use to provide fabrics with anti-graying properties in both aqueous and solvent-based laundering. The polycondensate of polyethylene glycol and terephthalic acid used in the present invention preferably has a molecular weight of 500 to 3,000. If the molecular weight is less than 500, the desired performance cannot be obtained, and if it is more than 3,000, the desired performance cannot be obtained. Although it is also affected by polycondensation, it becomes a polycondensate with poor solubility and is difficult to handle in practice. The degree of polycondensation between polyethylene glycol and terephthalic acid is suitably between 3 and 10. If the degree of polycondensation is less than 3, performance in terms of durability will be difficult, and if it is more than 10, the polymer will become insoluble in water, which will cause problems in use, although this will also be affected by the molecular weight of the polyethylene glycol used. Become. The amount of the polycondensate of polyethylene glycol and terephthalic acid used is preferably 0.1% to 10% owf based on the weight of the fiber. Polysiloxane resin is either dimethylpolysiloxane (average degree of polymerization 30-500) or methylhydrodiene polysiloxane (average degree of polymerization 10-80) having a hydroxyl group directly bonded to silicon at the end, or a mixture of both. Siloxane does not provide sufficient effects. When the average degree of polymerization of dimethylpolysiloxane is less than 30, the resin itself is unstable, and when it is more than 500, the viscosity is high, making it difficult to use in practice. Furthermore, methylhydrodiene polysiloxanes having an average degree of polymerization of 10 to 80 can be used, and those outside this range are difficult to use. It is desirable to use the polysiloxane resin in the present invention in an amount of 0.05% to 2% based on the weight of the fiber. If it is less than 0.05%, the effects of the present invention cannot be obtained, and if it is more than 2%, it may have an adverse effect on the slip property of the fabric. Among the melamine resins used, alkyl etherified methylol melamine resins have the best graying prevention properties and are advantageous in terms of stability, reactivity during processing, and the like. The amount of alkyl etherified methylolmelamine resin used should be 0.05% to 5% based on the weight of the fiber. If it is less than 0.05%, a sufficient graying prevention effect cannot be obtained, and if it is used more than 5%, the texture of the fabric becomes rough and hard, which poses a practical problem as a textile product. Regarding the texture of the fabric, it is possible to adjust the texture of the material to be treated by adjusting the proportions of the polycondensate of polyethylene glycol and terephthalic acid, the polysiloxane resin, and the melamine resin. To obtain a soft texture, use a large amount of the polycondensate of polyethylene glycol and terephthalic acid and polysiloxane resin, and conversely, to obtain a hard texture, use a large amount of melamine resin. In carrying out the present invention, it is desirable to use each catalyst in combination with the polysiloxane resin and the melamine resin in order to obtain a graying prevention effect that can withstand repeated water-based and solvent-based washings. Organic metal salts such as tin, lead or zinc are suitable as catalysts for polysiloxane resins, and organic amine salts or inorganic metal salts can be used as catalysts for melamine resins. In addition, polyester synthetic fibers tend to accumulate static electricity, which often causes problems in sewing operations unless treated with an antistatic agent.
According to the results of research conducted by the present inventors, the polycondensate of polyethylene glycol and terephthalic acid has antistatic properties, so it is possible to prevent static electricity without using an antistatic agent that has a negative effect on preventing graying. Textile products with high performance can be obtained. In order to apply the mixed emulsion of the polycondensate of polyethylene glycol and terephthalic acid, polysiloxane resin, and melamine resin used in the present invention to a polyester synthetic fiber fabric, the fabric is immersed in the mixed emulsion and squeezed uniformly, or The mixed emulsion may be sprayed onto the fabric, then dried and heat treated. Another method is to attach an emulsion of a polycondensate of polyethylene glycol and terephthalic acid to fibers in advance by an exhaustion method, dry and heat-treat the fibers, then immerse the emulsion in a mixed emulsion of polysiloxane resin and melamine resin, squeeze uniformly, or spray. or dipped in a polycondensate emulsion of polyethylene glycol and terephthalic acid and squeezed uniformly to dry.
After heat treatment, the same process may be performed again using a mixed emulsion of polysiloxane resin and melamine resin, or the order of applying the resin may be reversed, and any method of application may be used. . Drying may vary depending on the equipment and capacity, but may be performed at a temperature of about 100°C to 140°C for about 1 minute to 3 minutes. Heat treatment conditions vary depending on the resin used and each catalyst, but at a temperature of 150℃ to 200℃
It is sufficient to do this for 2 seconds to 2 minutes. Next, the present invention will be explained with reference to Examples, and the graying prevention performance in water-based and solvent-based washing was evaluated as follows. [Measurement in the laboratory] (1) Dry cleaning method (carbon stain test) Four samples (5 cm x 5 cm) were coated with carbon black.
0.01g, nonionic activator 1g, anionic activator 1
g, 0.2 g of water, 200 c.c. of perchlorethylene, and 10 steel balls (φ5 mm) in a pot with a lid.
Dry clean at 40°C for 30 minutes using a rounder-o-meter, then rinse the sample with fresh perchlorethylene only at 100 c.c. in a rounder-o-meter at 40°C for 10 minutes. The air-dried sample was used as a test sample. (2) Cleaning method with water: Clean 4 samples (5 cm x 5 cm) with 1 g of dirt base, detergent (mixture of sodium laurylbenzenesulfonate 1 g and sodium tripolyphosphate 1 g), water 200 c.c., and steel balls (φ5 mm) 10 Place the pieces in a pot with a lid and heat at 40℃ for 10 minutes using a rounder-o-meter.
After washing for 1 minute, rinse lightly with 40℃ water, add 200c.c. of 40℃ water to the same pot, and wash at 40℃ for 10 minutes.
Rinse for 10 minutes, then rinse with 200c.c. of water at 25℃ for 10 minutes.
After rinsing for a minute, the sample was dried in a tumbler at 60°C and used as a test sample. The stain sources used here are dry cleaning stains, artificial oil stains (stearic acid 15%, oleic acid 15%, beef tallow hydrogenated oil 15%, olive oil 15%, cetyl alcohol 10%).
%, cholesterol 5%, solid paraffin 25%)
are mixed at a ratio of 1:2. (3) Evaluation method (contamination rate) The reflectance (wavelength 480 nm) of the undry-cleaned cloth, the dry-cleaned cloth, and the unwashed cloth and the washed cloth with water was measured using a spectrophotometer. Reflectance of unwashed fabric and washed fabric, respectively.
The contamination rate was calculated using the following formula with R ₀ and R ₁ . Contamination rate (%) = R ₀ - R ₁ / R ₀ × 100 [Test at a local cleaning shop] When the processed fabric is spliced together and a cleaning test is conducted at a local cleaning shop, 3. (3) of [Laboratory Measurement]
The contamination rate was calculated using the same evaluation method as described in section. Example 1 A twill fabric woven using polyester processed yarn (150 denier/48 filaments) for the warp and weft was subjected to ordinary Relax scouring, dyeing (fluorescent white), and drying. The dried samples were immersed in baths of the following formulations 1 to 3, respectively, and squeezed uniformly at a squeezing rate of 80%. Next, after drying at 130°C for 2 minutes, heat treatment was performed at 170°C for 40 seconds.
Note that prescription 1 is a prescription for the method of the present invention,
Prescriptions 2 and 3 are cases where only one of the resins used in the method of the present invention was used for comparison with the present invention. Prescription 1 10 parts of polyethylene glycol and terephthalic acid polycondensate emulsion (A) (40% polycondensate of polyethylene glycol and terephthalic acid (average molecular weight 7000) with a molecular weight of 2000)
Aqueous solution) 0.2 parts of polysiloxane resin emulsion (B) (polysiloxane consisting of 20% dimethylpolysiloxane (average degree of polymerization 210) and 20% methylhydrogen polysiloxane (average degree of polymerization 40) having a hydroxyl group directly bonded to silicon at the end) Resin emulsion) Catalyst for polysiloxane resin Catalyst OZ (Catalyst for polysiloxane resin manufactured by Shin-Etsu Chemical Co., Ltd.)
0.02 parts methyl etherified trimethylolmelamine
0.6 parts Alkanolamine hydrochloride (40% aqueous solution, catalyst for melamine resin) 0.06 parts Water 89.12 parts Formula 2 Polycondensate emulsion of polyethylene glycol and terephthalic acid (A) 10 parts Formula 3 Polysiloxane resin (B) 0.2 parts Catalyst OZ 0.02 Partially methyl etherified trimethylolmelamine
0.6 parts Alkanolamine hydrochloride 0.06 parts Water 99.12 parts The graying prevention properties (contamination rate) and antistatic properties in water-based and solvent-based washing were measured for each of the obtained treated fabrics and are shown in Table 1. As is clear from Table 1, the method of the present invention had excellent anti-graying and antistatic properties. The method for measuring antistatic properties is as follows.
Samples dried at 105℃ for 1 hour at 20℃×40%RH
After leaving it for 48 hours in an atmosphere of
The half-life was measured under the condition of 10000V.

[Table] Example 2 A plain fabric woven from polyester processed yarn (150 denier/30 filaments) was subjected to usual scouring, dyeing (fluorescent white), and drying, and then immersed in a treatment bath of the following formulation 4, It was evenly squeezed with an aperture ratio of 80%. then
After drying at 120°C for 3 minutes, heat treatment was performed at 170°C for 40 seconds. After that, it is immersed in the treatment bath of prescription 5, and the squeezing rate is
Squeeze evenly at 80%, dry at 120℃ for 3 minutes, then dry at 170℃
Heat treatment was performed for 40 seconds. Formula 4 Polysiloxane resin (B) 0.2 parts Catalyst OZ 0.02 parts Methyl etherified trimethylolmelamine
0.7 parts Alkanolamine hydrochloride 0.07 parts Water 99.01 parts Prescription 5 Polycondensate emulsion of polyethylene glycol and terephthalic acid (A) 7 parts Water 93 parts The performance of the obtained treated fabric is shown in Table 2. As is clear from Table 2, the method of the present invention had excellent graying prevention properties. Moreover, antistatic properties were also good.

[Table] Example 3 The same polyester fabric as that used in Example 2 was immersed in a treatment bath of the following formulation 6, and the reduction rate was determined.
After squeezing uniformly at 80% and then drying at 130°C for 2 minutes, heat treatment was performed at 170°C for 30 seconds. Next, it was immersed in a treatment bath of formulation 7, squeezed uniformly at a squeezing rate of 80%, dried at 130°C for 2 minutes, and then heat-treated at 170°C for 30 seconds. Formula 6 Polycondensate emulsion of polyethylene glycol and terephthalic acid (A) 10 parts Water 90 parts Formula 7 Polysiloxane resin (B) 0.4 parts Catalyst OZ 0.04 parts Methyl etherified trimethylolmelamine
0.6 parts Alkanolamine hydrochloride 0.06 parts Water 98.9 parts The performance of the obtained treated fabric is shown in Table 3. As is clear from Table 3, the fabric obtained by the method of the present invention had excellent graying prevention properties. Also,
The antistatic property was also good.

[Table] Example 4 A plain fabric woven from polyester processed yarn (150 denier/30 filaments) was subjected to normal scouring and presetting, and then dyed (fluorescent white) using a treatment bath of the following formulation 8. It was stained at 130°C for 20 minutes and dried. Next, it is immersed in a treatment bath of prescription 9, and the squeezing rate is
Squeeze evenly at 80%, dry at 110℃ for 3 minutes, then dry at 180℃
Heat treatment was performed for 45 seconds. Prescription 8 Mika White ATN 1% owf Sunsalt #7000 1g / Acetic acid 0.2cc / Polyethylene glycol and terephthalic acid polycondensate emulsion (A) 15% owf Temperature x time: 130℃ x 20 minutes bath ratio: 1:20 Prescription 9 Polysiloxane resin (B) 0.2 parts Catalyst OZ 0.02 parts Methyl etherified methylolmelamine 0.5 parts Alkanolamine hydrochloride 0.05 parts Water 99.23 parts Table 4 shows the performance of the obtained treated fabric. As is clear from Table 4, the fabric obtained by the method of the present invention had excellent graying prevention properties. Also,
The antistatic property was also good.

【table】

Claims (1)

[Claims] 1. A polyester synthetic fiber fabric having an average degree of polymerization of 30 to 500 having a hydroxyl group directly bonded to silicon at the end.
dimethylpolysiloxane or average degree of polymerization 10~
0.05% or more of polysiloxane resin consisting of 80 methylhydrodiene polysiloxane alone or a mixture of both, based on the weight of the fiber, and an alkyl etherified methylol melamine resin based on the weight of the fiber.
A polycondensate of 0.05% or more and an average molecular weight of polyethylene glycol of 500 to 3000 and terephthalic acid with an average degree of polycondensation of 3 to 10 is attached to the fiber at a rate of 0.1% or more based on the weight of the fiber, and then heat treated at 150°C to 200°C. A method for producing a polyester synthetic fiber fabric having characteristics of preventing graying in water-based and solvent-based washing. 2. The constituent fibers of the fabric contain 0.05% or more of a polysiloxane resin based on the weight of the fibers, which is made of one or both of dimethylpolysiloxane and methylhydrodiene polysiloxane, each having a hydroxyl group directly bonded to silicon at the end, and an alkyl etherified methylolmelamine resin. A polyester synthetic fiber fabric having graying prevention properties, characterized by containing 0.05% or more of a polycondensate of polyethylene glycol and terephthalic acid based on the weight of the fibers, and 0.1% or more of a polycondensate of polyethylene glycol and terephthalic acid based on the weight of the fibers.