KR890000242B1 - Processing method of cotton textile - Google Patents

Abstract

A method for prepg. nonflammable cotton textile comprises (i) digesting cotton textile in nonflamming agent soln. (composed of (a) N-hydroxymethyl-3-(diethylphosphono)propion amides 25-50 % O.W.S., (b) nonionic surfactant 0.01-5 g/l, (c) polyethylenes softening agent 0.5-5 wt.% and (d) methyrols cross linking agent) in the presence of catalyst of formula NH2-(R1)-X and (ii) soaping with Na2CO3 soln.. Where R1=alkyl, aryl, alkylaryl or H, X=F, Cl, Br, I, n=1-20 integer.

Description

Durable flameproof processing method of cotton fabric

The present invention relates to a flame retardant processing method for imparting excellent durability flame retardant effect on cellulose fibers, especially cotton fabrics.

In general, cellulose-based fibers have excellent hygroscopicity and warmth, and are widely used for apparel for comfort and softness when worn.

However, the cellulose fiber is composed of flammable materials with high fire risk, which is one of the drawbacks of general polymer materials, and thus is weak in fire. To solve this drawback, it is urgently required to impart flame retardancy according to differentiation for each use. come.

Initially, the provision of flame retardancy has been mainly demanded in the case of carpets and carpets, but nowadays, it is widely required from work clothes, hospital and hotel interior materials, beddings, interior materials of aircrafts and aircraft interior materials. The methods for imparting flame retardancy to polymer fiber materials can be roughly divided into pre-treatment methods and post-treatment methods. As pre-treatment methods, 1) a method of obtaining a polymer having flame retardancy by copolymerizing a flame retardant monomer, and 2) There is a method of blending flame retardant material by spinning during spinning, and as a post-treatment method, 1) graft polymerization of the flame retardant material in a thread, a woven fabric, and a knitted fabric; and 2) during dyeing or other processing. Methods of penetrating and fixing flame retardant materials on fabrics have been known.

However, the pretreatment method of the above method is excellent in the flame retardant effect, but is used only for synthetic fibers and can not be applied to cotton fibers.

In addition, graft polymerization of flame retardant materials in post-treatment methods has been known for graft polymerization of vinyl monomers in which unsaturated compounds of phosphate esters are reacted with carbon radicals in cellulose.

However, such a chemical radical reaction (Rachical Reaction) is low because the reaction rate with cellulose must be reacted by using ultraviolet rays or electron beams in this case, it is limited in terms of equipment and industrial production has not been reached.

Therefore, among the post-treatment methods, the method of penetrating and fixing the flame retardant material on the fabric during dyeing or other processing is the most common method, and conventionally known techniques include flame retardant including N-metholol compound of dialkylphosphono carboxylic acid amide. There is a two-step processing method (Japanese Patent Laid-Open No. 47-37238) which simultaneously performs the first bath treatment for treating the fabric in the treatment liquid and the second bath treatment for the silicone emulsion treatment to improve the tear strength. In terms of flame retardancy and tear strength, good results can be obtained, but the process is complicated because it requires two times of processing, and the biggest drawbacks are the formation of flavin odor, hardening and discoloration of the touch.

MEANS TO SOLVE THE PROBLEM In order to solve the said fault, the present inventors earnestly researched and used a methirol type compound as a crosslinking agent in the flame retardant which consists of a high molecular compound containing phosphoric acid and nitrogen, and uses an amine compound as a reaction catalyst and a nonionic surfactant. It is immersed in the flame retardant liquid with dispersant and polyethylene compound as a softener for a certain time and then heat-treated. Soaping and removal of unreacted residue with sodium carbonate solution prevents poor durability, hardening of touch and deterioration of strength. The ease of processing can be achieved.

In the method of the present invention, by using a metholol compound having excellent crosslinking function as a crosslinking agent, the bonding strength between the flame retardant and the fiber is strengthened, and the durability is improved, and the reactivity is improved by using an amine compound having excellent reaction force as the reaction catalyst. Enhancement prevents tactile curing due to adhesion of the flame retardant to the fiber surface. By using a flame retardant composed of a high molecular compound containing phosphoric acid and nitrogen, the flame retardancy was remarkably improved by synergistic effects of phosphorus and nitrogen.

In addition, in order to improve flame retardancy in the conventional flame retardant processing method of cellulose fibers, the reaction is carried out under an ammonia gas atmosphere, which is restricted in the equipment. Processing in the usual resin processing machine was attained, obtaining the same effect as this improvement.

Hereinafter, the method of the present invention will be described in detail. The amine compound represented by the following formula (I) is used as a reaction catalyst, a flame retardant containing phosphoric acid and nitrogen is used at 25-50% OWS, and the methol compound is a crosslinking agent. 5-15% by weight of the flame retardant (weight ratio), polyethylene-based compound as a softener 0.5-5% (fiber weight ratio), non-ionic surfactant as a dispersant, cotton fabric was used in a flame retardant solution of 0.01-5 g / L After immersion, pre-dry at 110 ° C for 2 minutes, heat-treat at 160 ° C for 3 minutes, and finish by washing at 80 ° C for 5 minutes in sodium carbonate solution.

In the above formula

R ₁ : Alkyl group, Aryl group Alkyl Aryl group or hydrogen atom

X: halogen, fluorine, chlorine, bromine, iodine

n: integer of 1-20

In the present invention, the flame retardant includes N-hydroxymethyl-3- (diethylphosphono) propionamide, guanidine phosphate, ammonium phosphate, trichloroethylene phosphate, and amino-2-aminoethyl phosphate containing phosphoric acid and nitrogen. Most preferably, a compound of the N-hydroxymethyl-3- (diethylphosphono) propionamide-based compound is used. The flame retardant throughput is 25-50% (OWS) for the fiber to be treated, and the flame retardancy is less than 25% and the reactivity is poor at 50% or more, so there is no improvement in flame retardancy. Because it remains in a large amount, the initial feeling hardens.

As a crosslinking agent, a methirol-based compound is suitable, and the Tri-based compound is advantageous in terms of crosslinking function and feel than the Hexa-based compound. The proper use concentration of methylol compound is 5-15% (weight ratio) based on the amount of flame retardant used, and under 5%, crosslinking ability is insufficient, and at least 15% of unreacted crosslinking agent remains, resulting in formalin odor. It is also cured.

As the reaction catalyst, compounds such as NH ₃ , NH ₄ Cl ethanolamine, methylamine, NN-dimethylpropylenediamine, and ethylenediamine are used as the amine compound represented by the general formula (I). 5-20% (weight ratio) is appropriate for the amount of used, and below 5%, the sufficient effect as a reaction catalyst cannot be exerted, and at 20% or more, the crosslinking agent is decomposed, thereby decreasing the reactivity. The dispersing agent is suitable for nonionics considering the compatibility between flame retardants and other preparations. The proper use concentration is 0.01-5 g / L, and the dispersing agent cannot exhibit sufficient dispersing effect below 0.01 g / L. Inhibits the stability of the solution.

Softeners are suitable for the polyethylene-based compound in consideration of the softening effect and compatibility with other preparations. The proper use concentration is 0.5-5% (weight ratio) for the fiber to be treated, and below 0.5%, the feel of the fabric is processed. This is hardly improved, and at 5% or more, it can be seen that flame retardancy is lowered by excessive use of a softening agent.

Flame retardant processing of the present invention as described above is also possible in a padder (PADDER), tenter (TENTER) which is a conventional resin processing machine, the present invention will be described in detail with reference to the following examples. Flame retardancy shown in the Examples according to JIS L-1091 (45 ° method using a micro burner as a method of testing the combustibility of textile products), JIS L-0844 (using a household washing machine), and tensile strength according to KSK 0520.

Example 1

온도로 5분간 세척(Soaping)한후 다시 100℃온도로 2분간 건조하여 완성 하였다. 방염성의 평가 결과는 (표1)과 같으며, 강도, 촉감, 변색, 냄새 등의 물성 평가 결과는 (표2)와 같다.After dyeing the cotton fabric (weight: 200g / yd), it was immersed in the following treatment solution to pick up 70%, dried at 110 ° C for 2 minutes in a resin processing machine, and then heat-treated at 160 ° C for 3 minutes. . 80 ° in the sodium bicarbonate solution

After washing for 5 minutes at a temperature (Soaping) and dried again for 2 minutes at 100 ℃ temperature was completed. The results of evaluation of flame retardancy are shown in Table 1, and the results of evaluation of physical properties such as strength, touch, discoloration, and smell are shown in Table 2.

Comparative Example 1

Except for using the flame retardant in the treatment solution 20% by weight was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1) and (Table 2).

Comparative Example 2

Except that the flame retardant in the treatment liquid to 60% by weight was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 3

Except not using a crosslinking agent in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 4

Except for 10% by weight of the crosslinking agent in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 5

Except not using the amine compound as a reaction catalyst in the treatment liquid was processed in the same manner as in Example 1, flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 6

Except for 5% by weight of the amine compound as a reaction catalyst in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 7

Except for not using a softening agent in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 8

Except for 10% by weight of the softening agent in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

Comparative Example 9

Except not using a dispersant in the treatment solution was processed in the same manner as in Example 1, the flame resistance and physical properties evaluation results are shown in (Table 1), (Table 2).

[Table 1] Flame retardancy evaluation results

[Table 2] Property evaluation results

Claims (1)

N-hydroxymethyl-3- (diethyl phosphono) propionamide system containing phosphoric acid and nitrogen using an amine compound represented by the following formula (I) as a reaction catalyst using 5-20% (by weight) of a crosslinking agent The flame retardant was immersed in a flame retardant solution consisting of 25-50% OWS, 0.01-5 g / L of a nonionic surfactant, 0.5-5% of a polyethylene softener (weight ratio), and a known methirol-based crosslinking agent and washed with a solution of sodium carbonate (Soaping Durable flameproof processing method characterized in that.

In the above formula R ₁ : alkyl group, aryl group, alkylaryl group or hydrogen atom X: fluorine, chlorine, bromine, iodine as halogen element n: an integer from 1-20