JPS6278261A - Flame-proof processing agent for synthetic fiber material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to flameproofing agents for synthetic fiber materials, in particular polyester fibers or polyamide fiber materials.

BACKGROUND OF THE INVENTION Polybrominated compounds are known as one of the flameproofing agents for synthetic fiber materials. Since these compounds are solid at room temperature and water-insoluble, they have conventionally been used as aqueous dispersions.

As a method for producing an aqueous dispersion, for example, Japanese Patent Publication No. 53-8
As described in publications such as No. 840 and JP-A No. 57-137377, the current method is to mechanically pulverize powder using a pulverizer in water containing a dispersant or protective colloid to achieve dispersion. be.

However, in this method, a solid substance is simply physically pulverized by mechanical force, and there is a natural limit to the size of the particles that can be obtained, and particles with an average particle size of 1 μ or less are usually obtained. This was extremely difficult.

In the case of textile processing, the particle size of the processing agent is a very important factor. The smaller the particle size, the more desirable it is as a processing agent. Particularly when durability of the effect of the processing agent is desired, an increase in particle size is a fatal defect because the diffusion of the processing agent into the interior of the fiber is significantly reduced.

OBJECTS OF THE INVENTION The object of the present invention is to use a polybrominated organic compound to provide a flame retardant agent that can provide stable and durable flame retardant treatment to synthetic fiber materials.

Structure of the Invention The processing agent of the present invention is a) a polybrominated organic compound that is solid at room temperature, a) a phosphorus-containing compound that can dissolve the compound in a), and c) a compound represented by the following structural formulas I and II. at least one type of (where l is an integer of 1 to 3, n is an integer of 10 to 30,
represents Na or NHa).

Examples of the above compounds (a) include 1, 2, 5, 6, 9
°10-hexabromocyclododecane, 1,42.3.
4,5.6-hexabromocyclohebutane, 1,2,3
．． 4-tetrabromocyclooctane, 1,2.4.6-
Mention may be made of brominated cycloalkanes such as tetrabromocyclooctane, with 1,2,5,6,9.10-hexabromocyclododecane being particularly suitable.

In addition, examples of tris(1,3-
alkyl phosphates such as dichloropropyl) phosphate, tris(β-chloroethyl) phosphate, aryl phosphates such as triphenyl phosphate, tricresyl phosphate, tricylenyl phosphate, dimethylmethylphosphonate, diethyl N,N
-Bis(2-hydroxyethyl)aminomethylphosphonate and other phosphonic acid esters.

These phosphorus-based compounds can dissolve polybrominated organic compounds in monomolecular form at room temperature or by heating, and due to the synergistic effect of bromine and phosphorus, they provide excellent protection that cannot be obtained by simply using polybrominated organic compounds alone. It is possible to impart flame performance.

Further, examples of the compound c) include tristyrenated phenol/ethylene oxide adducts, sulfated tristyrenated phenol/ethylene oxide adducts, and the like. These compounds not only help the solubility of the polybrominated organic compound (a) in the phosphorus-based compound (a), but also improve the ability to uniformly apply the two types of compounds (a) and (a) onto the fibers. , these two types of compounds work to help diffuse uniformly inside the fiber through heat treatment.

Therefore, compared to conventional dispersions of polybrominated organic compounds, the effect of the finishing agent is more durable, the texture of the treated cloth is extremely soft, and there is less dusting (white powder on the surface of the treated cloth). The major advantage is that there is no whitening phenomenon that makes it look like it has been deposited.

The compounding ratio of compounds a), a), and c) is not particularly limited, but the weight ratio is 10 to 30%: 50 to 80%: 10 to
Desirably, it is 25%.

The flameproofing agent of the present invention can be diluted with a general solvent such as percrene or trichrene as it is, and processed into fibers by conventional padding, preliminary drying, and heat treatment. In addition, the flameproofing agent of the present invention can be easily emulsified by gradually adding water while stirring with a homomixer, etc., so it can be easily emulsified in a water-based manner like other general finishing agents. Processing using a dry-cure method is also possible. It is also possible to process by a so-called immersion process using a jet dyeing machine, a beam dyeing machine, a cheese dyeing machine, a package dyeing machine, etc.

In any case, the flame retardant of the present invention contains a polybrominated compound that is solid at room temperature dissolved in the form of flower molecules in a phosphorous solvent, so even when it is made into an aqueous emulsion, it is Compared to an aqueous dispersion produced by a mechanical pulverizer, the particle size is usually extremely small, approximately 0.3 μm or less, allowing for uniform and stable processing.

Next, the present invention will be explained in more detail with reference to Examples. In addition, the flame retardancy test of the processed cloth in the examples was carried out by the following method.

1) Flame retardancy test: JIS-1091D method (The larger the value, the better the flame retardancy.) 2) Washing method: JIS
L-1042 method 3) Dry cleaning method: JIS L-1018 method Example 1゜In a glass container equipped with a heating and stirring device, 15 g of 1.2,5,6゜9.10-hexabromocyclododecane, tris(β -chloroethyl) phosphate 55 g,) restyrenated phenol ethylene oxide 10 mole adduct 1
0 g was taken and gradually heated while stirring and kept at 120° C. for 15 minutes to obtain a transparent liquid. Next, the mixture was cooled to 90° C., 60 g of tetrachlorethylene was added, and then cooled to room temperature.

The obtained flame retardant agent (50% active ingredient of flame retardant) was further diluted 3 times with tetrachlorethylene to make the treatment liquid, a polyester fabric with a basis weight of 180 g/+" was padded and squeezed with a mangle. After the liquid (squeezing ratio: 60%), it was dried at 130°C for 5 minutes, and then heat-treated at 170°C for 2 minutes.

Comparative Example 1 A polyester fabric was processed in exactly the same manner as in Example 1, except that the same amount of tetrachlorethylene needles was used instead of tris(β-chloroethyl) phosphate.

Comparative Example 2 A polyester fabric was processed in exactly the same manner as in Example 1, except that the same amount of tetrachlorethylene was used instead of the 10 mole tristyrenated phenol/ethylene oxide adduct.

Table 1 shows the results of the H flammability test of the work fabrics obtained in Example 1 and Comparative Example 1.2.

Table 1 Processing of Example 1 according to the present invention Right center, Karoe upper blade
After washing and dry cleaning, all three samples exhibited excellent flame retardancy and had a good texture. On the other hand, the processed fabric of Comparative Example 1, which was treated with the compound (1) of the present invention (11"G), was generally lacking in flame retardancy. The processed fabric of Comparative Example 2, which was processed without using any of the above methods, had some imperfections in flame retardancy, suggesting that uniform adhesion of the flame retardant was not obtained.

In addition, the washing and dry cleaning durability is also inferior to that of the method of the present invention.

Example 2 L2, 5.6°9 in a glass container with heating and stirring device
．． Collect 10 g of 10-hexabromocyclododecane, 5 g of tricresyl phosphate 5 (Ig), 20 mole adduct of restyrenated phenol and ethylene oxide, and 7 g of the sulfate ammonium salt of the 20 mole adduct of restyrenated phenol and ethylene oxide. While stirring, the mixture was gradually heated and kept at 120°C for 15 minutes to obtain a transparent liquid. Next, this was cooled to 90°C, and while stirring was continued, 30g of water was gradually poured in. After stirring for another 15 minutes, the mixture was gradually cooled to room temperature to form a milky white powder with a particle size of 0°2 to 0.3μ. An emulsion was obtained (59% flame retardant active ingredient).

Using this emulsion, a polyester wiping cloth was treated by the dipping method as described below.

1) Wiping cloth: 100% polyester fabric (basis weight 200g/
2) Processing machine: HI, = DI dyeing tester 3 manufactured by Todoroki Sangyo Co., Ltd.
) processing conditions.

Actual Tt Emulsion of Example 2 17% o, wJ.

Temperature: 30°C After processing for 30 minutes, simply wash 3 sections with cold water and dry (110°C x 3
minutes), a flame retardant test was conducted. The results are shown in Table 2.

Table 2 The processed fabric of Example 2 according to the present invention was made flame retardant, and the effect persisted even after washing and dry cleaning.

Effects of the Invention The flame retardant of the present invention contains a) a polybrominated organic compound)
When used in combination with a phosphorus compound and c) a compound represented by the above structural formula I and/or II, it can be provided in the form of a solution, making it very easy to handle, in either liquid or aqueous dispersion form. Even when used in containers, uniform processing into synthetic fiber materials is possible.

In addition, in the processing using the flame retardant of the present invention,
and c) the synergistic effect of the three types of compounds provides superior flame retardant performance that cannot be obtained with polybrominated organic compounds alone;
The texture of the processed cloth is also excellent.

Patent applicant: Meisei Chemical Industry Co., Ltd. 1 person from outside the company: Shin Minoru Ken

Claims (2)

[Claims] (1) A) Polybrominated organic compound that is solid at room temperature, B) B)
A phosphorus-containing compound capable of dissolving the compound, c) The following structural formula:
At least one type of compound represented by I and II ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ (I) ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ (II) (However, l is an integer from 1 to 3, and n is Integer from 10 to 30, X
A flame retardant agent for synthetic fiber materials, characterized in that it contains the following three components: (2) The above compounds a), b) and c) in a weight ratio of 1
The flameproofing agent according to claim 1, containing the flame retardant in a ratio of 0 to 30%: 50 to 80%: 10 to 25%.