KR20150141345A - Method of Flame-Retardant Finish for Fiber Materials Comprising Cotton - Google Patents

Abstract

The present invention relates to a method for processing a flame-retardant fiber product comprising at least 80% of cotton and, more specifically, to a processing method for directly providing flame retardant properties for a fabric containing cotton or a fiber product composed of the fabric/ The method comprises a flame-retardant composition manufacturing step, a fiber product immersing and picking-up step, a first drying step, a curing step, a washing step, and a second drying step.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a flame-

FIELD OF THE INVENTION The present invention relates to a flame-proofing method for a textile product comprising a face, and more particularly, to a method of imparting flame-retardant properties directly to fabrics or clothing containing faces.

Flameproofing is a process that loses the ability of a textile to propagate fire. It is a process that allows it to be self-extinguished by burning only when it comes in contact with flames and removing flames.

Currently, most of the industrial flame retarding garments are mainly made of modacrylic fiber, which is a mixture of Aramid (trade name: Kevlar), DuPont flame retardant fiber, and Lenzing FR fiber, Lenzing. However, the modacrylic fiber material is expensive, so it is not economical, it is difficult to dispose of it, and toxic gas is generated.

With the growing interest in environmental protection, there is an increasing demand for natural fibers that are more environmentally friendly and easier to dispose of in the textile sector. Of these natural fibers, cotton fibers are one of the most commonly used fibers, but they are flammable compared to other fibers and are required to be flame retardant. When a cotton fiber comes into contact with a flame, decomposition is initiated by heat and levoglucosan is produced and decomposed into a flammable gas, which reacts with oxygen in the air and proceeds to a burning process. Flame retarding of this cotton fiber is to change the combustion process. The combustion process is known to be capable of changing the phosphorus-containing material, which is synergistic when used with a nitrogen-containing material.

Regarding flame retarding processing, U.S. Patent No. 3,556,840 discloses a technique for flame-retarding a cellulose material. This patent describes the use of phosphopropionamide and an acid catalyst to impart flame retardancy to the cellulosic material.

In Korean Patent No. 171899, 3- (dimethylphosphono) -propionate methylolamide is impregnated into fabric and cured by heating with an auxiliary reactant such as melamine formaldehyde condensate to produce flame retardant cotton fabric having durability to some extent in washing And the like.

However, these patents disclose techniques for imparting flame retardancy to fabrics such as cotton fabrics. In general, flameproofing has a technical limitation in that flameproofing is limited depending on the kind of the fabric, because the flameproofing fabric uses a flameproof fabric and a flameproof fabric.

Therefore, there are a lot of limitations on flame-retarding clothes and bedding that have been used in the past.

An object of the present invention is to provide a method of flame-treating a fiber product containing 80% or more of cotton in a simpler, more effective and environmentally friendly manner. It is also an object of the present invention to provide a method capable of directly flame-proofing not only fabrics like fabrics but also textile products such as curtains made of such fabric.

The above-mentioned problems are solved by a method for producing a flame retardant composition, comprising: preparing a flame retardant composition containing a melamine resin, a flame retardant, a softener, a penetrant and phosphoric acid; Dipping the fiber product containing 80% or more of cotton in the flame retardant composition 1 to 2 times and picking up the fiber product at a pick-up rate of 70 to 90%; First drying the fiber product; Curing the dried fiber product; Washing the cured fiber product with water mixed with a soda ash and a detergent in a weight ratio of 2: 1; And a second step of drying the washed fiber product.

Preferably, the flameproof composition comprises 1 to 10% by weight of a melamine resin, 1 to 10% by weight of a softener, 0.001 to 5% by weight of a penetrant, 30 to 70% by weight of a flame retardant, 1 to 5% And may contain residual water.

Further, preferably, the flame retardant may be N-hydroxymethyl-3-dimethylphosphonopropionamide.

In addition, the primary drying step may be performed at 90 ° C to 130 ° C for 10 to 20 minutes.

Also, the curing step may be performed at 170 ° C to 180 ° C for 1 to 10 minutes, or at 150 ° C for 5 to 20 minutes.

According to the processing method of the present invention, it is possible to carry out flame-proofing on fabric products such as existing clothes and bedding products, as well as fabrics without replacing the fabric or deforming the product.

BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a process diagram for explaining a flame-retarding process of a textile product including a face according to the present invention;

All technical terms used in the present invention have the same meaning as commonly understood by those of ordinary skill in the related art unless otherwise defined. Also, preferred methods or samples are described in this specification, but similar or equivalent ones are also included in the scope of the present invention.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flame-retarding process of a textile product comprising a face of the present invention. Fig.

Referring to FIG. 1, the method for flame-treating a textile article of the present invention comprises the steps of (S11) producing a flame retardant composition, (S12) dipping a fiber product into a flame retardant composition, (S13) and curing the dried fiber product (S14); Washing the dried fiber product (S15); And secondary drying (S16).

First, a flame retardant composition is prepared (S11). The flameproofing composition can be prepared by adding a melamine resin, a softening agent, a penetrating agent, a flame retardant, and phosphoric acid to water sequentially and stirring. Preferably 1 to 10% by weight of a melamine resin, 1 to 10% by weight of a softener, 0.001 to 5% by weight of a penetrant, 30 to 70% by weight of a flame retardant, 1 to 5% by weight of phosphoric acid, do. More preferably, it contains 4 to 7% by weight of a melamine resin, 3 to 5% by weight of a softener, 0.1 to 1% by weight of a penetrant, 45 to 65% by weight of a flame retardant, 2 to 3% by weight of phosphoric acid and residual water.

As the melamine resin, a known product can be used, and hexamethylol melamine or melamine-formaldehyde resin can be preferably used. In the present invention, MR-6 product of Sun Synthesis Co., Ltd. was used. The melamine resin causes the flame retardant to react with the cellulose and adhere well to the fiber product. The melamine resin is preferably used in an amount of 1 to 10% by weight based on the total weight of the flameproofing composition. More preferably, 4 to 7% by weight can be used. When the content of the melamine resin is less than 1% by weight, the flame retardant is difficult to react with cellulose. When the content of the melamine resin is more than 10% by weight, the fabric becomes stiff.

The softener may be polyethylene wax, silicone softener, or the like. The softening agent may be used in an amount of 1 to 10% by weight based on the total weight of the flameproofing composition. More preferably 3 to 5% by weight.

The flame retardant may be an organophosphate type, and preferably N-hydroxymethyl-3-dimethyl phosphonopion amide. The flame retardant may be used in an amount of 30 to 70% by weight, preferably 45 to 65% by weight, based on the total weight of the flameproofing composition. When the flame retardant is added in an amount of less than 30% by weight, the flame retardant effect on the fabric is low, and when it exceeds 70% by weight, the fabric becomes stiff after flame retardant processing.

The penetrating agent may be a nonionic surfactant. Preferably, polyoxyethylene, polyoxyethylene alkyl ether, or polyoxyethylene alkyne ether can be used. In the present invention, DJ-P1020 product of Daejeong Trading Co., Ltd. was used. The penetrating agent is preferably used in an amount of 0.001 to 5 wt%, more preferably 0.1 to 1 wt%, based on the total weight of the flameproofing composition. When the penetrant is less than 0.001 wt%, the flame retardant is not well dispersed in the flame retardant composition, and when it is more than 5 wt%, the flame retardant may be contained excessively in the fiber product.

The phosphoric acid may be used in an amount of 1 to 5% by weight based on the total weight of the flameproofing composition. More preferably 2 to 3% by weight. Phosphoric acid is preferably administered to the last layer when preparing a flame retardant composition. The phosphoric acid can be added after diluting it in cold water by quantifying the required amount. Phosphoric acid plays a role as a catalyst to make the cellulose of the fiber product react well with the flame retardant.

Next, the fiber product is immersed in the flame retardant composition (S12). In the present invention, the fiber product preferably comprises a fabric or a knitted fabric having a surface of 80% or more. More preferably, the cotton content may be 82% or more. When the content of cotton in the fabric is less than 80%, the flame-retardant processing is not effectively performed. The fiber product of the present invention includes not only the fabric including the face but also the garment and the fabric product comprising the fabric. The fabric product includes bedclothes, curtains, tablecloths and the like.

The fiber product can be immersed in the flame retardant composition for 5 to 10 minutes, and the immersion step can be carried out once or twice for effective immersion. After immersion, you can pick up from 70% ~ 90% pick-up rate on pad mangles. The pick-up rate may vary depending on the weight or composition of the fabric. The pick-up rate can be increased by increasing the immersion time of the flame-retardant composition in the fiber product, that is, by slowing the padding speed.

Next, primary drying is performed (S13). The primary drying may be performed in a drier at 90 to 130 ° C for 10 to 20 minutes. Preferably, the drying temperature is 110 占 폚. If possible, the primary drying can be done in vacuum. The primary drying removes excess moisture from the fiber product so that the reaction between the flame retardant and the fiber product in the flame retardant composition occurs efficiently. Since the flame retardant composition is prepared by diluting a component such as a flame retardant agent into water to remove the flame retardant agent, the concentration of the flame retardant agent in the fiber product is increased to efficiently perform the reaction and fixation of the flame retardant agent. In the primary drying, the drying temperature is preferably 90 to 130 ° C, and more preferably 110 ° C. If the primary drying temperature is less than 90 ° C, the flame retardant does not adhere well to the fiber product, and if it exceeds 130 ° C, a dye transfer problem occurs. The dried textile product may be further subjected to a partial vacuum process (Air extraction).

Then, the dried fiber product is immediately cured (S14). The curing step is a kind of heat treatment process. The dried fiber product is cured at 170 to 180 ° C for 1 to 10 minutes, and more preferably, cured at 175 ° C for 1 minute. The run can be treated at 150 ° C for 5 to 20 minutes. In the curing stage, the flame retardant reacts with the cellulose in the fiber product to impart flame resistance to the fiber product. Also, the flame retardant is bonded to the cellulose of the fiber product by the heat treatment and is not easily removed during washing, thereby exhibiting almost permanent characteristics. If the curing step is not successful, the fiber product will absorb moisture, and if the residual water content is excessive, it may cause a mildew.

Next, the dried fiber product is washed (S15). The washing step is to wash the dried fiber product by mixing the soda ash (Na ₂ CO ₃ anhydride) and the detergent in water at a weight ratio of 2: 1. The water temperature is preferably 45 to 50 ° C. Then wash 3 ~ 4 times until clear water comes out. The soda ash can be used in an amount of 20 to 30 g / L based on 1 L of water, and 1 to 1.5 g / L of the cleaning agent can be used based on 1 L of water. A commercially available laundry detergent may be used as the detergent. At this stage, phosphoric acid contained in the flameproofing composition can be removed. It is desirable to wash the textile within 24 hours after the curing step. The soda ash can be added as an alkaline material for neutralization of textile products. The soda ash serves to prevent hydrolysis of the textile product during storage. After washing, the fiber product preferably has a pH of 8 to 9.

Finally, the washed textile can be dried naturally or dried in a dryer at 60 ° C for 20 minutes (S16). The dried product is finally ironed and finished with flame-retarding treatment.

The flame-retarded fiber product by the above-described method can maintain flame retardancy even in repeated washing. However, it is preferable to rinse with an acidic product during washing or avoid steam ironing in order to maintain flame proofing property for a long time.

Hereinafter, the present invention will be described in detail with reference to Examples, but the scope of the present invention is not limited by these Examples.

Production Example 1 - Preparation of Flame Retardant Composition

65 g of a melamine resin (MR-6, Sun Synthetic Co.), 45 g of a silicone emulsifier (DJ-MS300N, Daejeong Trading Co.), 5 g of a penetrating agent (DJ-P1020, Daejeong Trading Co.) Methyl-3-dimethylphosphonopropionamide) was added to prepare a composition. 25 g of phosphoric acid (80%) was added to a small amount of water and diluted. The flame-retardant composition was added to the above composition, and the remaining amount of water was added thereto to prepare a flame retardant composition in an amount of 1 L, followed by stirring for 30 minutes.

Example  One

100% cotton fabric (40's Interlock FR Jersey, 260 g / m < ² >) was immersed in the flame-retardant composition prepared in Preparation Example 1 for 5 minutes. The dipped sample was picked up at a 75% pick-up rate from the padding mangles and dehydrated. After dehydration, it was dried in an electric dryer (primary drying) at 100 ° C for 10 minutes and then cured in an electric dryer at 175 ° C for 10 minutes. The dried sample was immersed in a solution prepared by adding 0.2 g / L of soda ash and 0.1 g / L of water to 1 L of water, followed by washing 3 to 4 times until clear water was generated. After that, it was naturally dried (second drying) and ironed with an electric iron to complete the final flame retarded cotton fabric.

Example  2

100% cotton fabric (30's Twill, 128 g / m ² ) refined and bleached was immersed in the flameproof composition prepared in Production Example 1 for 5 minutes. The dipped sample was picked up at a 75% pick-up rate from the padding mangles and dehydrated. After dehydration, it was dried in a 110 ° C electric dryer (primary drying) for 10 minutes and then cured in an electric dryer at 180 ° C for 5 minutes. The dried sample was immersed in a solution prepared by adding 0.2 g / L of soda ash and 0.1 g / L of water to 1 L of water, followed by washing 3 to 4 times until clear water was generated. After that, it was naturally dried (second drying) and ironed with an electric iron to complete the final flame retarded cotton fabric.

Experimental Example 1 - Results of flame resistance measurement

The flammability of the cotton fabrics prepared in Examples 1 and 2 was measured by ASTM F1506: 2010a. The flame retardancy was measured before washing and after 25 times of washing.

The washing conditions were washed 25 times based on AATCC 135: 2012 (Test No. (3) (IV) A (iii) Machine Wash Permanent, Press Cycle at 49 ± 3 ° C, Tumble Dry Permanent Press).

The test requirements are as follows.

- After Flame: Up to 2.0 seconds

- CHAR Length: Up to 152 mm

- Burnong Behavior: No Melting and Dripping

The measurement results are shown in Table 1.

After Flame Time
(second) After Glow Time
(second) CHAR Length
(mm) Burning Behavior Before washing 25 times
After washing Before washing 25 times
After washing Before washing 25 times
After washing Melting Dripping Example 1 slope
(Warp) 0 0 0 0 87 102 No No Weft
(Weft) 0 0 0 0 90 108 Example 2 slope
(Warp) 0 0 0 0 78 102 No No Weft
(Weft) 0 0 0 0 81 105

As can be seen in Table 1, the flame retarded fabric products prepared in Examples 1 and 2 satisfied all flame retardancy requirements.

Experimental Example 2 - Wash fastness measurement

The washing fastness of flame retarded samples was measured according to ASTM F 1506: 2010a. Test conditions were AATCC 61: 2010 (Test No. 2A, 45 minutes machine wash at 49 ± 2 ° C, 0.15% AATCC Wob Detergent Solution with 50 Steel Balls). The measurement results are shown in Table 2 below. As shown in Table 2 below, it can be seen that the washing fastness is very good as fourth grade.

Wash fastness Color change (based on cotton fabric) 4 Example 1 4 Example 2 4

Experimental Example 3 - Measurement of shape stability for washing

Tensile Strength (ASTM 5034: 2009, C.R.E. Method) was measured after five washes to determine the shape stability of the laundry. The measurement results are shown in Table 3 below. In Table 3 below, (+) means expansion and (-) means contraction.

After washing 5 times (%) Tensile strength (N) Example 1 slope -0.8 450 Weft -0.8 206 Example 2 slope -0.8 333 Weft -0.8 135

As shown in Table 3, it was confirmed that only about 0.8% was shrunk and almost no deformation was observed.

Claims (6)

A flame-proofing method for a fiber product containing 80% or more cotton,
A flame retardant composition comprising a melamine resin, a flame retardant, a softener, a penetrant and phosphoric acid;
Dipping the fiber product containing 80% or more of cotton in the flame retardant composition 1 to 2 times and picking up the fiber product at a pick-up rate of 70 to 90%;
First drying the fiber product;
Curing the dried fiber product;
Washing the cured fiber product with water mixed with a soda ash and a detergent in a weight ratio of 2: 1; And
A method of flame-treating a textile product, comprising the step of secondary drying the washed textile product. The flame-retardant composition of claim 1, wherein the flame-retardant composition comprises 1 to 10% by weight of a melamine resin, 1 to 10% by weight of a softener, 0.001 to 5% by weight of a penetrant, 30 to 70% , And a remaining amount of water. The method according to claim 1, wherein the flame retardant is N-hydroxymethyl-3-dimethylphosphonopropionamide. The method according to claim 1, wherein the primary drying step is performed at 90 ° C to 130 ° C for 10 to 20 minutes. The method according to claim 1, wherein the curing step is performed at a temperature of 170 ° C to 180 ° C for 1 to 10 minutes. The method according to claim 1, wherein the curing step is performed at 150 ° C for 5 to 20 minutes.

Images