JP2000328445A - Flame-proof finishing of polyester fiber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To perform durable flame-proof finishing of a polyester fiber with little deterioration of light-fastness by adding an emulsion composition containing a resorcinol bis(diphenyl phosphate) to a dyeing bath for a polyester fiber. SOLUTION: A resorcinol bis(diphenyl phosphate) expressed by formula is dispersed in water in the presence of 2-30 wt.% (based on the resorcinol compound) nonionic surfactant such as polyoxyalkylene alkylphenyl ether and/or anionic surfactant such as an alkylsulfate salt. The obtained emulsion composition is added to a dyeing bath for a polyester fiber and a polyester fiber is dipped in the bath and subjected to the flame-proof treatment simultaneously with dyeing treatment at >=80 deg.C for 2-60 min to achieve the flame-proof finishing of the polyester fiber.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flame-retardant method for durable polyester fiber, which hardly reduces light fastness and durable.

[0002]

2. Description of the Related Art Conventionally, an aqueous dispersion of hexabromocyclododecane (JP-B-53-8840) has been known as a flame retardant treatment agent for polyester fibers. However, it has been pointed out that halogen-based flame retardants generate dioxin during waste incineration, and development of a flame-retardant processing method for non-halogen-based compounds has become a major issue.

[0003]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a polyester fiber with a flame-retardant property which has a small decrease in light fastness and is durable by post-processing using a compound containing no halogen atom. It is.

[0004]

Means for Solving the Problems The inventors of the present invention have made intensive studies to solve the above-mentioned problems, and as a result, have obtained a polyester fiber having a good durability with a small decrease in light fastness and a high durability by post-processing. Have been found, and the present invention has been achieved. That is, the method for flame-retarding polyester fibers of the present invention comprises resorcinol bis (diphenyl phosphate)
(Hereinafter, abbreviated as RDP) is emulsified and dispersed in water in the presence of a surfactant to prepare an emulsified composition, and the emulsified composition is added to a dye bath, and simultaneously adsorbed on polyester fibers at the same time as dyeing. It is characterized by the following. Also, the present invention relates to R
In the presence of a nonionic surfactant and / or anionic surfactant in an amount of 2 to 30% by weight based on DP, an emulsified composition in which RDP is emulsified and dispersed in water is prepared, and the emulsified composition is prepared. It is also characterized in that the polyester fiber is added to a dye bath, the polyester fiber is immersed in the obtained dye bath, and treated at a temperature of 80 ° C. or more for 2 to 60 minutes. Of course, it is possible to impart good flame retardancy to polyester-based fibers even when treated under the same conditions as dyeing without adding a dye. An emulsified composition is prepared by emulsifying and dispersing in water, the emulsified composition is added to a bath having a composition not containing a dye, and the polyester fiber is immersed in the obtained treatment bath to a temperature of 80 ° C. or higher. This is a flame-retardant processing method for polyester-based fibers characterized in that the treatment is performed for 2 to 60 minutes.

[0005] When RDP is emulsified and dispersed in water, a nonionic surfactant and / or an anionic surfactant is used as a surfactant. As a nonionic surfactant,
Examples include polyoxyalkylene alkyl phenyl ether, polyoxy alkylene alkyl ester, polyoxy alkylene alkyl ether, polyoxy alkylene tristyryl phenyl ether, castor oil alkylene oxide adduct, polyoxy alkylene alkyl amine ether, and the like. Most preferred are polyoxyalkylene tristyryl phenyl ether and castor oil alkylene oxide adduct. These nonionic surfactants may be used alone or in combination of two or more. Examples of the anionic surfactant include an alkyl sulfate salt, an alkyl sulfonate salt, an alkyl phosphate salt, an alkyl aryl sulfate salt, an alkyl aryl sulfonate salt, a polyoxyalkylene alkyl ether sulfate salt, a polyoxyalkylene tristyryl phenyl ether sulfate salt, and a polyoxyalkylene. Alkyl ester phosphate salts, polyoxyalkylene alkyl ether carboxylate salts, polycarboxylate salts, funnel oil, petroleum sulfonates, alkyl diphenyl ether sulfonate salts and the like, but alkyl aryl sulfonate salts, polyoxyalkylene tristyryl phenyl ether sulfate salts Most preferred. Further, these anion activator salts include alkali metal salts, alkaline earth metal salts, ammonium salts, organic amine salts and the like.
These anionic surfactants may be used alone or in combination of two or more.

The larger the amount of the nonionic surfactant used, the higher the R
It is effective for emulsifying and dispersing DP, but has a large slow-dyeing effect and has an adverse effect on dyeing. When used, its content is preferably 2 to 30% by weight based on RDP.

The larger the amount of the anionic surfactant used, the higher the R
It is effective for emulsification dispersion of DP and dispersion of dye, but generally foams greatly, and there is a detrimental effect on fiber treatment due to foaming. When used, 2 to 30% by weight based on RDP is preferable.

[0008] The RDP emulsified composition in the flame-retardant processing method of the present invention does not necessarily require a solvent, but may be included for keeping the emulsified composition uniform or for improving emulsification. Representative solvents include methyl alcohol, ethyl alcohol, isopropyl alcohol, benzene, xylene, toluene, ethyl acetate, dimethylformamide, petroleum ether, chloroform, ethylene glycol, butyl cellosolve, 1,5-pentanediol, ethylene carbonate, propylene carbonate , Propylene glycol, dipropylene glycol, triethylene glycol, triethylene glycol dimethyl ether, pentaethylene glycol monobutyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, tetraethylene glycol dimethyl ether, propylene glycol monomethyl ether, dipropylene glycol Thing Although ether and the like, ethylene glycol, butyl cellosolve are preferred. These solvents may be used as a mixture of two or more kinds. The amount used is preferably from 0 to 20% by weight based on RDP.

The form of the polyester fiber used in the present invention is not particularly limited as long as it is a fiber product such as a yarn, a woven or knitted fabric, a nonwoven fabric, a rope, or the like. In addition, natural fibers, regenerated fibers, semi-synthetic fibers, and other synthetic fibers may be mixed with such polyester fibers as long as the effects of the present invention are not impaired.

Other compounds other than RDP include other flame retardants,
A deodorant / antibacterial agent, a softener, an SR agent, a lightfastness improver, an antistatic agent, and the like may be previously attached or adsorbed to the polyester fiber. Moreover, you may make it adsorb | suck simultaneously with the process of this invention.

The amount of RDP adsorbed is 2% or more, preferably 4 to 8%, based on the weight of the polyester fiber. 2
If it is less than 8%, the flame retardant effect may be insufficient, and if it exceeds 8%, the flame retardant effect is not further improved, so that it is not economical.

In the present invention, when RDP is adsorbed on a polyester fiber, RDP emulsified and dispersed in water in the presence of a surfactant is added to a dye bath, and the polyester fiber is immersed in the bath. The treatment is performed at a temperature of 80 ° C. or higher, preferably 110 ° C. or higher, and more preferably 130 ° C. or higher for a period of several minutes to 60 minutes. When the flame-retardant processing method of the present invention is used, the adsorption efficiency of RDP from the bath is 70 to 9
It is as high as 5%. When the polyester fibers are treated under such conditions, the RDP is adsorbed not only on the fiber surface but also inside the fibers one by one, and flame retardancy excellent in washing resistance, dry cleaning resistance and the like can be obtained. In addition, when the hexabromocyclododecane dispersed in water in the presence of a surfactant is adsorbed on polyester fibers at the same time as the dyeing, the sunlight fastness of the dyed material decreases, but as in the present invention, When RDP emulsified and dispersed in the presence of a surfactant is similarly adsorbed, the fastness to sunlight hardly decreases.

Further, in the case of the flame-retardant processing method of the present invention in which RDP is adsorbed on polyester fibers, there is an advantage that the exhaustion of the disperse dye is hardly hindered and the dyeing of the polyester fibers can be carried out simultaneously. .

As another method for adsorbing RDP, there is a pad method, more specifically, a pad-dry-cure method or a pad-dry-steaming method. Performance cannot be obtained. On the other hand, when the adsorption method of the present invention is used, stable flame retardancy can be provided.

In the present invention, when the flame retardant treatment of the polyester fiber is treated with a phosphorus compound such as RDP, no dioxin is generated as in the case of the halogen compound during waste incineration, which is preferable from the viewpoint of eco-friendliness.

[0016]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be further described below with reference to examples, but the present invention is not limited to these examples. Parts in Examples are parts by weight, and% means% by weight. In addition,
The performance values shown in Examples and Comparative Examples were measured by the following methods.

(Flame retardancy) JIS L 1091 D method. (Washing and dry cleaning durability) JIS L 1
091 The washing and dry cleaning methods described in Textile Product Flame Retardancy Test Methods. This procedure was repeated five times. (Light fastness) JIS L 0842 (carbon arc light, black panel temperature 83 ° C x 100 hours, urethane foam backing)

Example 1 A 300 g / m ² polyester fabric was scoured by a conventional method.
It was dried and heat set at 180 ° C. for 2 minutes. This fabric is used as a disperse dye [Sumikaron Red SE-RPD (Sumitomo Chemical)]
2% owf dispersion leveling agent [Disper N-700 (manufactured by Meisei Chemical)]
0.5 g / l of a water-emulsified dispersion (treatment agent A) of RDP according to the following formulation was treated in a dye bath containing 10, 20, and 30% owf at a bath ratio of 1:10 at 130 ° C. for 30 minutes. In the formula (a), reduction washing, water washing, and drying were performed at a bath ratio of 1:20, 80 ° C. × 20 minutes.

(Treatment agent A) RDP 500 parts Polyoxyethylene (20 mol addition) tristyryl phenyl ether 50 parts Polyoxyethylene (20 mol addition) tristyryl phenyl ether sulfate salt 20 parts Water 430 parts Total 1000 parts

Comparative Example 1 A polyester fabric was processed in exactly the same manner as in Example 1 except that 10, 20, and 30% owf of an aqueous dispersion of hexabromocyclododecane having the following formulation (treatment agent B) was used.

(Treatment agent B) Hexabromocyclododecane 500 parts Castor oil ethylene oxide 20 mol adduct 50 parts Lauryl alcohol sulfate sodium salt 20 parts Water 430 parts Total 1000 parts

Formula (a) Minex WTS (Meishei Chemical detergent) 2 g / l Hydrosulfite conc 1 g / l soda ash 2 g / l sodium tripolyphosphate 2 g / l

The results of measuring the flame retardancy and light fastness of these are shown in Table 1.

[0024]

[Table 1]

The work cloth of Example 1 according to the present invention shows extremely excellent durable flame retardancy after treatment drying, 5 washings and 5 times dry cleaning, and also has good light fastness. Met. On the other hand, the processed cloth of Comparative Example 1 using the aqueous dispersion of hexabromocyclododecane, which is a conventional technique, is not generally excellent in flame retardancy and also inferior in light fastness to the method of the present invention. Was.

Comparative Example 2 In order to compare the method of treating the same polyester fabric used in Example 1 simultaneously with dyeing (Example 1) with the pad method, 10, 20, 30, 40% of the treating agent B was used. Pad the solution, pick up 75%, dry 110 ° C x 2 minutes,
Cure 180 ° C. × 1 minute, reduction washing, water washing and drying with a liquid obtained by removing the hydrosulfite conc from the prescription (a).
The results of measuring the flame retardancy of these are shown in [Table 2].

[0027]

[Table 2]

Compared with the dyeing method according to the present invention, the work cloth by the pad method was inferior in flame retardancy after 5 times of washing and 5 times of dry cleaning.

Example 2 The exhaust dyeing method for polyester fibers is classified into an acidic or neutral dyeing method (Example 1) and an alkaline dyeing method. The same polyester fabric used in Example 1 was mixed with a disperse dye [Sumikaron Blue E-FBL (Sumitomo Chemical)] and a 1% owf dispersion leveling agent [Disper N-700 (Meisei Chemical)] 0.5 g / l. , An alkaline agent for alkaline dyeing [Olinax AM-80 (manufactured by Meisei Chemical Co., Ltd.)] 2 g / l, a self-emulsifying RDP regulator (treatment agent C) having the following formulation:
5, 11.1 and 16.6%, treated in an alkaline dyeing bath containing 16.6% owf at a bath ratio of 1:10 at 130 ° C. for 30 minutes. Reduction washing, water washing, and drying were performed.

(Treatment agent C) RDP 900 parts Polyoxyethylene (20 mol addition) tristyryl phenyl ether 30 parts Polyoxyethylene (20 mol addition) tristyryl phenyl ether sulfate 70 parts Total 1000 parts

COMPARATIVE EXAMPLE 3 Exactly the same as Example 2 except that treating agent B of Example 1 was used in an amount of 10, 20, and 30% owf so that the amount of the active ingredient was almost the same as that of treating agent C of Example 2. To process the polyester fabric. The results of measuring the flame retardancy of these are shown in [Table 3].

[0032]

[Table 3]

The work cloth of Example 2 according to the present invention was subjected to the alkali dyeing method. However, after the treatment and drying, after 5 times of washing and 5 times of dry cleaning, the fabric had extremely excellent durable flame retardancy. Indicated. On the other hand, the work cloth of Comparative Example 3 using the aqueous dispersion of hexabromocyclododecane, which is a conventional technique, was not generally excellent in flame retardancy.

[0034]

According to the present invention, RDP emulsified and dispersed in water in the presence of a surfactant is dyed and adsorbed on polyester fibers at the same time as dyeing, so that the decrease in light fastness is small and the durability is high. And stable flame-retardant polyester fiber, and at the same time, because this emulsified dispersion does not contain halogen atoms, dioxin is generated when the treated polyester fiber is discarded and incinerated. It is also preferable from the viewpoint of environmental protection.

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Tomonori Hata 1 Nakanishacho, Nishikyogoku, Ukyo-ku, Kyoto, Kyoto Prefecture Inside (72) Inventor Hidetoshi Asai 1-Nakagashizawa, Nishikyogoku, Ukyo-ku, Kyoto, Kyoto Chemical industry Co., Ltd. F term (reference) 4H028 AA35 BA04 4L033 AA07 AB01 AC05 BA14 BA39 CA48

Claims (3)

[Claims] 1. The following chemical formula: The emulsified composition is prepared by emulsifying and dispersing resorcinol bis (diphenyl phosphate) in water in the presence of a surfactant, and adding the emulsified composition to a dye bath, and simultaneously dyeing the polyester fiber. A method for flame-retarding polyester fibers, wherein resorcinol bis (diphenyl phosphate) is adsorbed. 2. Emulsifying resorcinol bis (diphenyl phosphate) in water in the presence of a nonionic surfactant and / or an anionic surfactant in an amount of 2 to 30% by weight based on resorcinol bis (diphenyl phosphate). Preparing a dispersed emulsified composition, adding the emulsified composition to a dye bath, immersing the polyester fiber in the obtained dye bath, and treating at a temperature of 80 ° C. or higher for 2 to 60 minutes. The method for flame-retarding polyester fibers according to claim 1. 3. An emulsified composition is prepared by emulsifying and dispersing resorcinol bis (diphenyl phosphate) in water in the presence of a surfactant, and adding the emulsified composition to a dye-free bath. A method for flame-retarding polyester fibers, wherein the polyester fibers are immersed in the obtained treatment bath and treated at a temperature of 80 ° C. or higher for 2 to 60 minutes.