JPH08209537A - Flexible and durable flame-retardant cloth - Google Patents

Abstract

PURPOSE: To produce a flame-retardant cloth having softness and high washing resistance without deteriorating the characteristic features of cellulosic fiber. CONSTITUTION: This flame-retardant cloth having softness and excellent washing resistance is produced from a blended cloth composed of a chlorine-containing synthetic fiber having increased flame retardancy and a natural cotton fiber at a weight ratio (synthetic/natural) of 30/70 to 70/30 by treating the cloth with a phosphorus-containing flameproofing agent to an extent to apply 0.1-3.0wt.% of the agent in terms of phosphorus to the cloth.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cloth composed of chlorine-containing synthetic fibers and cellulosic fibers, which makes use of the characteristics of soft cellulosic fibers and has excellent flame resistance and durability against washing. It is used for interior goods such as clothing, curtains, upholstery, and bedding.

[0002]

2. Description of the Related Art Many flame-retardant cloths made of cellulosic fibers have been introduced. However, in the conventional cellulosic flameproof fabric, since the flameproofing agent comes off by washing and the degree of flame retardancy decreases, the flameproofing agent is previously added in a large amount of 20 to 50% by weight based on the fiber weight. It was used for the above, and was treated in anticipation of the loss of the flameproofing agent. Further, in order to improve the durability of washing, a fiber finishing agent such as a melamine type is used together with a flameproofing agent in a large amount of 5 to 10% by weight or more based on the weight of the fiber.

[0003] For example, as a compounding example of a treatment liquid in the case of subjecting a conventional cellulosic fiber to a flameproof treatment, a phosphorus-containing flameproofing agent 20 to 50%, a hexamethylolmelamine finishing agent 5 to 10%, a softener 3% phosphoric acid Such as 2% catalyst 1%. These were all used weight% based on the weight of the fiber, and it was normal to use such a large amount.

The flameproof fabric is usually subjected to the steps of preparing a treatment liquid, dipping, squeezing, drying and curing,
Then, it is obtained by neutralizing, washing and drying. The cloth obtained by such a process has a problem caused by the use of a large amount of a processing agent, such as a hard touch, discoloration of color, odor, residual formalin, etc. There was a problem. In addition, in order to reproduce the desired imparting of flame retardancy and to avoid the above-mentioned obstacles, it is necessary to perform processing with great care, and the cost of the fabric has always been a problem.

Further, as to the flame-retardant washing durability, as described above, the flameproofing agent generally tends to fall off every time washing is repeated, and the flame retardancy tends to decrease. In anticipation of this, the above-mentioned phosphorus-containing flameproofing agent and finishing agent must be used in an increased amount. The treatment with these processing agents has been devised to fix them chemically or physically, but when a large amount of a fixing agent is used, the fabrics are touched and rubbed against each other during washing, Due to this action, it is always in a state where falling out easily occurs.
An example of a washing method for evaluating the wash resistance is AATC.
C TEST METHOD 135-1987, DIMENSIONAL CHANGES IN AUT
OMATIC HOME LAUNDERING OF WOVEN AND KNITFABRICS.
There are 7 TEST PROCEDURE A 7,2,3 DUMMY PIECES,
It is presumed that the use of the dummy pieces (DUMMY PIECES) here was set in consideration of the fact that the fabrics touch each other during washing. Therefore, the use and adhesion amount of the phosphorus-containing flameproofing agent is
It can be said that a method capable of exhibiting a flame retardant effect with a small amount is preferable.

As described above, it is extremely difficult to impart a flame-retardant property, which is flexible and has durability to washing, to cellulosic fibers typified by wood cotton, etc. Was long-awaited.

[0007]

SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a flame-retardant cloth which is flexible and has good washing durability without impairing the features of cellulosic fibers.

[0008]

The above object is to treat a mixed cloth of chlorine-containing synthetic fibers containing 1 to 50% by weight of an antimony compound and cellulosic fibers with a phosphorus-containing flameproofing agent. 0.1 to 0.1% phosphorus to the cloth
It is achieved by treating to 3.0% by weight.

Here, as the antimony compound,
Antimony oxides such as antimony trioxide and antimony pentoxide are mentioned. These compounds are contained in the chlorine-containing synthetic fibers in an amount of 1.0 to 50% by weight, preferably 5 to 25% by weight, more preferably 10 to 20% by weight.

As the chlorine-containing synthetic fiber, for example, a polymer whose constituent is 40 to 70% by weight of acrylonitrile, 60 to 30% by weight of vinyl monomer containing chlorine, and a sulfonic acid group-containing unit amount There is a polymer consisting of 0 to 3% by weight, but the polymer may be polyclar.

Further, as the cellulosic fiber, for example, natural cotton fiber, ramie, linen, or recycled fiber viscose rayon staple or filament, or polynosic, cupra staple or filament, etc. can be mentioned. .

Further, in the present invention, the mixed cloth of the chlorine-containing synthetic fiber containing the antimony compound and the cellulosic fiber is a cloth obtained by blending, twisting, and twisting these fibers, The weight ratio of the former and the latter is 10: 9
0 to 70:30, preferably 30:70 to 70:
30 is good. Further, these fabrics may be mixed with a small amount of other fibers, for example, 3 to 10% by weight of polyester, polyamide, aramid, etc.
It may be a woven fabric, a knitted fabric, or a non-woven fabric.

The phosphorus-containing flameproofing agent includes, as typical examples, conventionally known flameproofing agents for the following cellulosic fibers. is not. That is, as a phosphorus-containing flameproofing agent for cellulosic fibers, for example, JSDCVO
Representative examples are: ○ N-methyloldimethylphosphonopropionamide ○ Tetrakis (hydroxymethyl) phosphonium chloride ○ Amidophosphazene compounds, which are introduced in LUME 99 JULY / AUGUST 1983 191. The effect of these phosphorus-containing flameproofing agents on cellulosic fibers is to suppress afterflame and dust by promoting carbonization of the flame contact part confirmed in the combustion test and to reduce the carbonization length and carbonization area. This shows the features of the flameproofing agent.

The amount (treatment amount) of these flameproofing agents containing phosphorus with respect to the target mixed fabric is such that the phosphorus content weight% is 0.1 to 3.0. 0.2 to 1.0 is preferable. Even more preferably, 0.4 to 0.8 is good.

The phosphorus content weight% (hereinafter,
It is written as P%. ) Is a fluorescent X-ray analyzer SEA20
01 Using a tabletop type (Seiko Denshi Kogyo Co., Ltd.) and 99.9% diammonium phosphate reagent (Wako Pure Chemical Industries, Ltd.), create a calibration curve as shown in FIG. 1 for each target fabric in advance. And carried out. Further, regarding the formulation using phosphoric acid, the value obtained by subtracting (phosphoric acid usage amount × 31/98) from the measured P% was defined as P%.

Further, in the present invention, the treatment liquid containing a fiber finishing agent as a main component can be used for the treatment together with the above phosphorus-containing flameproofing agent. Examples of the finishing agent for the cellulosic fibers used in this case include melamine resins such as Sumitex resin M-3 or M-6 (both Sumitomo Chemical Co., Ltd.) and dimethylol dihydroxyl ethylene urea type, for example, FIXAPRET. CPJ (BASE) can be mentioned,
Polycationic dyes, fixing agents such as Sunfix P
When AC700 (Sanyo Kasei Co., Ltd.) is used, a processing agent such as a softening agent, an antistatic agent, a water repellent agent, or the like which has a function is also used in combination. These are used after confirming the liquid stability in advance.

Next, the outline of the treatment with the flameproofing agent containing phosphorus in the present invention will be described. First, a treatment liquid containing the above-described flameproofing agent containing phosphorus and, if necessary, a finishing agent is prepared. Next, the target cloth is dipped in this treatment liquid and squeezed using a mangle. The fabric is thoroughly dried at 100 ° C and then 150-160 ° C.
Cure at. Next, wash (depending on the treatment liquid,
Neutralization and washing are carried out, and the treatment is completed by thoroughly drying at 100 ° C.

In addition, in addition to the above, evaluation of flexibility (evaluation of bending resistance), washing conditions and evaluation of flame retardancy will be described in detail in the following examples.

[0019]

EXAMPLES The present invention will be shown below by Examples, but the present invention is not limited thereto.

[Example 1] 1. Preparation of original fabric 1-1. Preparation of chlorine-containing synthetic fiber containing antimony compound Acrylonitrile (AN), vinylidene chloride (VD), and sodium styrene sulfonate (SSS) were polymerized using the respective monomer weight ratios of 50/49/1. A resin was obtained. This was dissolved in acetone, antimony trioxide (Sb ₂ O ₃ ) was added, and a solid solution containing 20 wt% of Sb ₂ O ₃ was prepared. Next, hole diameter 0.09mmφ
Wet spinning was performed from the spinneret by a conventional method to obtain a fiber bundle having a single fineness of 2 denier. Subsequently, an oil agent and a crimp were added and cut into 38 mm to obtain the fiber. 1-2. Fabrication of a cloth for mixing the above chlorine-containing synthetic fiber and a cellulosic fiber A mixing weight ratio of the above chlorine-containing synthetic fiber and cotton cotton is 50/5.
No. 0, and this was spun and twisted using a known cotton spinning system, and the 26th yarn (26/2) and the 18th yarn (18 /
A blended yarn of 2) was obtained. Next, using 26/2 as a warp and 18/2 as a weft, and using a dobby fiber machine, a twill fabric (2/1 twill) was obtained. This 2/1 twill was subjected to hair-burning, refining, bleaching, and mercerizing in accordance with the usual steps of a wooden cotton cloth, and then dried and set to obtain a cloth original cloth of Example 1 as described below. (Fabric fabric) Twill fabric (2/1 twill) Weight: 312 g / m ² Warp: 26/2, density 78 threads / inch Weft: 18/2, density 50 threads / inch

2. Manufacture of the base fabric of the comparative example The base fabric of the comparative example was a 2/1 twill of 100% wood cotton, but was carried out in the same manner as the example fabric. The difference between the example fabric base fabric and the comparative example fabric base fabric in this step is that caustic soda flakes were 5 g / liter at 85 ° C. in the example.
In contrast to the scouring and bleaching treatment in Example 1, the comparative example treatment was carried out by treating the same flakes at 20 g / liter at 100 ° C. However, this difference is caused by the suitability of the chlorine-containing synthetic fiber for alkali, and does not affect the essence described below.

3. Treatment with a Flame Retardant Containing Phosphorus Using the cloth original fabrics of the above-mentioned Examples and Comparative Examples, treatment with a treatment liquid containing a flame retardant finishing agent containing compounded phosphorus shown in Table 1 below as a main component was performed. .

[0023]

[Table 1]

3-1. Method of Treatment After preparing the treatment liquids (1-A) to (1-D) shown in Table 1 above, the cloth original fabric of the above-mentioned example was treated with the treatment liquids (1-A) and (1-B), respectively. The fabric raw fabric of the comparative example was treated with the treatment liquid (1-
C) and (1-D), respectively, squeezed with a mangle (pickup 80%), dried at 130 ° C. for 10 minutes, and immediately cured at 150 ° C. for 10 minutes. PH7 with a solution containing soda ash
Neutralize and treat at 85 ° C for 5 minutes, then wash with warm water at 85 ° C,
5 minutes and 40 degreeC, 5 minutes were performed. Drying is performed with a mungle after dehydration with a pin tenter at 120 ° C. for 10 minutes, and a treatment (P-treated) fabric mainly containing a flameproofing agent containing phosphorus from (1-A) to (1-D). Got

[0025] 4. Combustion test The combustion test method is the US test method, NFPA 1975 Standard.
on Station / Work Uniforms for Fire Fighters 4-2 F
lame Resistance Test "Flame Resistance of cloth; Ve
rtical "of Federal Test Method Standard 191A (hereinafter referred to as FTMS 191A).

5. Laundry test The washing test method is the American test method, AATCC 135 3-IV-
Carry out according to A iii, no wash (W-O), wash 2
The sample piece of 5 times (W-25) and 50 times of washing (W-50) was created. Dummy pieces (DUMMY
PIECES) was added.

[0027] 6. Evaluation of flexibility The flexibility test was carried out by JIS L 1096 6.19 Bending flexibility A method (cantilever method).

Table 2 shows the evaluation results of the durable flame-retardant fabrics of the above-mentioned Examples and Comparative Examples.

[0029]

[Table 2]

(Confirmation of Effect) As is clear from Table 2,
As a result of the combustion test by FTMS 191A, the fabrics of Examples were treated with the treatment agent (1-A) and the treatment agent (1-B) to obtain W.
The flame-retardant effect of reducing the carbonization length by P treatment (5.1 → 3.9 inches) withstanding -25 and W-50 was shown. On the other hand, the fabrics of the comparative examples treated with the treatment liquids (1-C) and (1-D) show the case of total burning (carbonization length 12.0 inches), and the P weight is about 5 times the weight of the examples. %, It did not show durability despite treatment.

Further, as a result of evaluation of flexibility by the bending resistance A method, 51-53 mm was shown in the example, but 84-90 mm was shown in the comparative example. This result is similar to the tactile sensation determination, confirming the flexibility of the example.

Example 2 Using the resin shown in Example 1, 1.5 denier fiber containing 10% by weight of antimony trioxide (Sb ₂ O ₃ ) and 38 mm, the same content as shown in Example 1 was used. Was manufactured along with. The chlorine-containing synthetic fiber containing the antimony compound and cotton cotton were mixed and mixed at a weight ratio of 30:70, and the resulting fabric was woven, fried, scoured, and bleached to obtain the following fabric. (Fabric fabric) Plain woven fabric Weight: 160 g / m ² Warp: 20 /-Density, 62 threads / inch Weft: 20 /-Density, 62 threads / inch

The above cloth fabric was treated with a flameproofing agent containing phosphorus using the treatment liquids (2-A) to (2-E) shown in Table 3 below.

[0034]

[Table 3]

On the other hand, as a comparative example, a wooden cotton cloth conforming to the standards and processing procedures of the above-mentioned examples was used and treated with the treatment liquid (2-F) shown in Table 3. The phosphorous treatment weight percent of each fabric was measured by fluorescent X-ray. Table 4 shows the P weight% relative to the weight of the fabric and the evaluation results of the combustion test.

[0036]

[Table 4]

(Confirmation of effect) As is clear from Table 4,
In the case of a blended lightweight fabric (Example) of 30% chlorine-containing synthetic fiber containing 10% by weight of Sb ₂ O ₃ and 70% cotton cotton, even if the P% by weight is 0.1, the durability against washing is exhibited, and further, P% by weight
Of 0.3 and 0.6 showed good wash durability and flame retardancy. On the other hand, in Comparative Example, both W-0 and W-25 had insufficient flame retardancy. In addition, the touch was good for all the sample pieces.

[Example 3] Using the chlorine-containing synthetic fibers containing the antimony compound shown in Example 1, the following cloths having different ratios of mixed cotton cotton cloths are shown in Table 5. It was created and a combustion test was conducted. (Fabric fabric) Plain fabric Weight: 161 g / m ² Warp: 30/2, Density 60 yarns / inch Weft: 30/2, Density 40 yarns / inch Phosphorus weight treatment% (P% by weight) 0.6 The combustion test was carried out with FTMS 191A, and the number of washings was once (W-1). The results are shown in Table 5.

(Confirmation of effect) Mixed ratio of wood cotton 70 to 30
%, All of them showed good flame retardancy, and the touch was soft and good. On the other hand, 100% of the cotton tree of Comparative Example
The flame retardancy of the fabric was insufficient. In addition, the reference example 0
% Fabric showed good flame retardancy, but the reduction in carbonization length was
It did not reach the examples.

[0040]

[Table 5]

[0041]

INDUSTRIAL APPLICABILITY As described above, the flame-retardant cloth according to the present invention is obtained by mixing the cloth containing the chlorine-containing synthetic fiber and the cellulosic fiber with the phosphorus-containing flameproofing agent, and By treating it so that its weight is 0.1 to 3.0% by weight, it is flexible while maintaining the characteristics of cellulosic fibers such as wood cotton, and has good flame resistance with good washing durability. Utilizing the flame retardancy with excellent washing durability, it is widely used in the field of flame retardant fiber products such as clothing, curtains, upholstery such as upholstery and bedding, which require flexibility and washing durability. It can be used.

[Brief description of drawings]

FIG. 1 is a graph showing a calibration curve of phosphorus content.

Claims (4)

[Claims] 1. A cloth for mixing chlorine-containing synthetic fibers containing an antimony compound in an amount of 1 to 50% by weight and a cellulosic fiber is used as a flameproofing agent containing phosphorus, and the weight of phosphorus is 0.1 to the weight of the cloth. A flexible and durable flame-retardant fabric, which is treated so as to be 3.0% by weight. 2. The durable flame-retardant cloth according to claim 1, wherein the cloth for mixing chlorine-containing synthetic fibers and cellulosic fibers is obtained by mixing, twisting, and weaving these fibers. 3. The durable flame-retardant fabric according to claim 1 or 2, wherein the weight ratio of the chlorine-containing mixed fiber and the cellulosic fiber is 10:90 to 70:30. 4. The durability according to claim 1, wherein the treatment with a flameproofing agent is performed with a treatment liquid containing a flameproofing agent and a finishing agent as main components. Flame-retardant cloth.