KR102050566B1 - Flameproof method of cellulose fabric, and RAYON goods manufactured of cellulose fabric of the same - Google Patents

Abstract

The present invention relates to a flame-retardant finish method of cellulose-based fabrics. More specifically, the present invention relates to a method for flame-retardant finish of cellulose-based fabrics without reducing physical properties of products; and cellulose-based fabrics flame-retardant finished by the method.

Description

Flameproof processing method of cellulose-based fabric and cellulose-based fabric flame-proof processed by the same method {Flameproof method of cellulose fabric, and RAYON goods manufactured of cellulose fabric of the same}

The present invention is a method for flame retardant processing by a specific flame-retardant processing technology of cellulose-based (cotton, linen, hemp, lami, etc.) fibers, including cellulose or cellulose-based fibers and regenerated rayon fibers It relates to a flame retardant product.

Cellulose fibers such as aramid, cotton, and rayon are one of the combustible materials that are easily burned by flame or heat and have fire propagation ability in various applications such as clothing, bedding, furniture, etc. Various flame control laws and regulations have been enacted, and consumers' interests and demands for flame retardant processing are gradually increasing. In general, the flame retardant treatment of the fiber by post-processing gives durable self-extinguishing property by using an organic phosphorus flame retardant or halogen flame retardant. However, halogen-based flame retardants are increasingly being used because they can adversely affect the human body and the environment due to their toxicity and corrosive gases such as halogen acids during combustion. Therefore, in recent years, research on flame retardant processing using inorganic particles or organophosphorus flame retardants has been actively conducted.

The organophosphorus flame retardant does not generate a large amount of corrosive gas during the combustion process unlike the halogen flame retardant because it acts as a condensation mechanism to change the pyrolysis mechanism to reduce the calorific value and increase the amount of residual carbide.

THPC flame retardant alone does not react well with cellulose fibers and does not form polymers.However, THPC flame retardants form non-soluble polymers inside cellulosic fibers when they are treated with materials containing active hydrogens such as amides or amines. It has the advantage of making aramid and cotton blend products that can have a fire retardant effect. Sodium phosphate monohydrogen has been reported to be effective as a catalyst when treating THPC flame retardants with amides containing active hydrogens such as urea and cyanamide, and Franklin et al. Have been described as THPC-Urea-sodium hydrogen phosphate flame retardants. The results of the study showed that the treated aramid and cotton blend products significantly reduced the production of Levoglucosan compared to the aramid and cotton blend products treated with other flame retardants.

In general, the process using THPC flame retardant provides flame retardant to the cellulose fabric by high temperature heat treatment of the flame retardant and resin. Significantly decreases in the characteristics of the stiffness and the touch hardening, such as problems of the cellulose-based fabrics using THPC flame retardant process has been a considerable difficulty.

Korea Patent Publication No. 10-2013-0017757 (2013.02.20) Korean Laid-Open Patent No. 10-2006-0002681 (2006.01.09)

After a long study, the inventors have conducted a high-speed flame retardant treatment of knitted fabrics and / or fabric fabrics of cellulose-based (cotton, linen, hemp, lami, etc.) and / or recycled rayon fibers, while greatly improving productivity and preventing the strong degradation of the fabric. The present invention was completed by knowing the optimum flame retardant treatment conditions, the optimal flame retardant concentration, and the like, which can prevent the decrease.

The present invention for solving the problem relates to a flame retardant processing method of a cellulose-based fabric, after flame-retardant cellulose-based fabric, or a cellulose-based fabric comprising a cellulose-based fiber and regenerated rayon fibers, padding the fabric. 1 step of processing; Step 2 of drying the padded fabric; Curing the dried fabric with an amine curing agent using a high speed curing device; 4 steps of oxidizing the cured fabric; 5 steps of washing the oxidized fabric; And six steps of drying the washed fabric.

In addition, another object of the present invention is to provide a cellulose-based fabric product flame-retardant processed by the above method.

Unlike conventional cellulose-based fabric products (knitted fabrics and / or fabrics), the flame retardancy, strength and fastness of washing are rapidly reduced by repeated washing, the cellulose-based fabric products produced by the flame retardant processing method of the present invention are flame retardant, strength by repeated washing. And washing fastness is very little or no effect.

1 is a rear view of the curing apparatus used in the present invention.
2 is a side view of the curing device used in the present invention.
Figure 3 is expressed by the chemical formula a preferred example of the compound that serves as a flame retardant of the high-speed flame-resistant fabric of the present invention.

The term "cellulose-based fabric" used in the present invention blends not only cellulose-based fabric of 100% cotton, but also cellulose fibers including one or more selected from aramid fibers, linen fibers, flax fibers, hemp fibers and rayon fibers. It is meant to include knitted fabrics or fabrics containing more than 90% cotton.

Hereinafter, the present invention will be described in more detail.

Flame retardant processing method of the cellulose-based fabric of the present invention after the flame-retardant cellulose-based fabric, or a cellulose-based fabric comprising a cellulose-based fiber and regenerated rayon fibers, a step of padding the fabric (padding); Step 2 of drying the padded fabric; Curing the dried fabric with an amine curing agent using a high speed curing device; 4 steps of oxidizing the cured fabric; 5 steps of washing the oxidized fabric; And six steps of drying the washed fabric.

The cellulose-based fabric of step 1 is a cellulose fiber; Or 50 to 99.9% by weight of cellulose-based fibers and the remaining amount of regenerated rayon fibers, including knitted fabric or woven fabric.

After immersing the cellulosic fabric in the padding solution, the padding mangling treatment may be performed at a pressure of 2.5 to 3.5 kgf and a speed of 1.0 to 30.0 m / min, followed by squeezing treatment.

And, the padding solution is 30 to 45% by weight of flame retardant containing a Tetrakis Hydroxymethyl Phoshonium Chloride (THPC) -urea condensate, 3.0 to 4.5% by weight of glyoxal resin, 0.05 to 0.5% by weight of the penetrant and the balance It includes water, preferably 35 to 45% by weight of the flame retardant, 3.5 to 4.5% by weight of glyoxal resin, 0.05 to 0.35% by weight of the penetrant and the remaining amount of water.

The flame retardant in the padding liquid component may be a flame retardant including a THPC-urea condensate, and a general flame retardant may be used, and (HOCH ₂ ) ₃ PClCH ₂ NHCONHCH ₂ PCl (CH ₂ OH) ₃ may be used. Can be. The flame retardant may be an equivalent ratio of THPC and urea of 1.8 to 2.2: 1, specific gravity of 1.28 to 1.30 (25 ° C.), and a phosphorus content of 14 to 15 wt% per pure solid.

And, if the flame retardant content in the total weight of the padding liquid is less than 30% by weight, it may be difficult to secure long-term flame retardancy due to repeated washing, and even if the flame retardant content is used in excess of 45% by weight, there is no increase in the flame retardant effect, It is good to use within the above range because it may fall.

The glyoxal resin in the padding liquid component serves as a crosslinking agent for crosslinking the flame retardant to the cellulose-based fabric, and is contained with the THPC (Tetrakis Hydroxymethyl Phoshonium Chloride) -urea condensate and the total weight of the padding liquid. If the resin is less than 3.0% by weight of cross-linking with the flame retardant in the cellulose-based fabric may not be well secured flame retardant, more than 4.5% by weight is used excessively, tearing steel due to glyoxal resin in the cellulose-based fabric In addition, the cellulose-based fabric has a problem that the roughness increases, the flexibility decreases, and the long-term fastness due to repeated washing is rather deteriorated.

The penetrant in the padding liquid component serves to smooth the swelling of the cellulosic fibers, but may be a general one used in the art, but preferably Triton X-100 (Triton X-100), concentration of 10Be or less At least one selected from caustic soda and monohydric alcohol may be used, and more preferably, at least one selected from triton X-100 and caustic soda having a concentration of 10 Be or less may be used. In addition, when the penetrant content is less than 0.05% by weight of the total weight of the padding liquid, swelling may not occur well and there may be a problem, and when it exceeds 0.5% by weight, there may be a problem of overswelling. good.

In addition, the padding liquid is adjusted to pH 5.2 to 6, preferably pH 5.4 to 5.8 after mixing the flame retardant, penetrant and water, wherein the pH of the padding liquid is less than 5.2 of the cellulose-based fabric There may be a problem that the cellulose fibers are embrittlement, if the pH exceeds 6 there may be a problem that the flame retardant effect is lowered. As the alkaline solution used for pH adjustment, it is preferable to use one alkali solution selected from among sodium hydroxide aqueous solution and KOH.

Next, the drying in two steps may be performed by tentering for 60 seconds to 120 seconds at 130 to 150 ° C, preferably for 70 seconds to 100 seconds at 132 to 148 ° C. At this time, if the temperature of the flame retardant to be less than 140 ℃ is not enough to increase the moisture content, or the drying time may be too long, if the temperature exceeds 150 ℃ drying of the flame retardant completely occurs and the moisture content is rather Since there may be a problem of becoming too low, it is preferable to perform the drying by tending under the above temperature. The blended product, which has been subjected to two stages of drying, is treated with 10 to 50%, preferably 20 to 40%, when the moisture pick-up (%) is measured based on Equation 1 below.

[Equation 1]

Moisture content (Wet pick up,%) = (Weight of cellulose-based fabric before drying-Weight of cellulose-based fabric after drying) ÷ Weight of cellulose-based fabric after drying × 100 (%)

Next, the third step is curing by dipping or spraying the amine-based curing agent to the dried cellulose-based fabric, 1.5 per 1 mole of phosphorus (P) of the flame retardant treated on the cellulose-based fabric The flow rate of the amine curing agent, that is, the spray injection amount, is cured by adjusting the flow rate of the amine curing agent so as to crosslink with the amine compound at a molar ratio of ˜2.2 moles, preferably 1.95 to 2.05 moles.

The crosslinking reaction between the flame retardant and the amine compound in the chamber occurs in a short time within 1 to 15 seconds, using the specific curing device. It can be carried out by dividing by car.

Referring to the high speed curing apparatus used in the present invention in detail.

1 is a rear view showing a high speed curing device according to the present invention, Figure 2 is a side view of the curing bone foot device.

The curing device is largely the chamber 110; Cellulose-based fabric inlet 120; Curing agent supply unit 130; First curing agent injection unit 140; Cellulose-based fabric transfer unit 150; A second curing agent injection unit 160; Cellulose-based fabric discharge unit 170; And a third curing agent 180, wherein the chamber 110 is enclosed.

The cellulose-based fabric inlet 120 is provided at one side of the chamber 110 and serves to introduce the cellulose-based fabric into the interior. The cellulose-based fabric introduced into the cellulose-based fabric inlet 120 is a cellulose-based fabric which has been padded with a flame retardant and dried.

The curing agent supply unit 130 is provided outside the chamber 110 and serves to supply the curing agent into the chamber 110.

The curing agent supply unit 130, the curing agent supply tank 131, the vaporizer 132, the curing agent storage tank 133, the curing agent supply pipe to supply the curing agent into the chamber 110 It consists of 134.

The curing agent supply tank 131 receives the curing agent which is a liquid and serves to supply the contained curing agent.

The curing agent storage tank 133 serves to store the curing agent.

The curing agent supply pipe 134 serves to supply the curing agent from the curing agent storage tank 133.

The first curing agent injection unit 140 is provided on one side of the chamber 110 adjacent to the cellulose-based fabric inlet 120, the cellulose-based introduced by the cellulose-based fabric inlet 120 Spraying the curing agent supplied from the curing agent supply unit 130 to the lower portion of the fabric serves to primary cure the cellulose-based fabric.

The first curing agent injection unit 140 is composed of a curing agent inlet pipe 141 and the injection nozzle 142.

The curing agent inlet pipe 141 is supplied with the curing agent supplied from the curing agent supply pipe 134, is installed in the chamber 110, the width of the cellulose-based fabric perpendicular to the transfer direction of the cellulose-based fabric Direction is installed.

The injection nozzle 142 is installed on the curing agent inlet pipe 141 spaced apart at regular intervals in the direction of the width of the cellulose-based fabric, the curing agent introduced from the curing agent inlet pipe 141 of the cellulose-based fabric It is sprayed to the bottom and consists of a plurality.

As such, the present invention allows the curing agent to be directly sprayed on a cellulose-based fabric, thereby curing the curing agent. It has the advantage of improving the flame retardant properties of the cellulose-based fabric by doubling the fixing force adsorbed on the product.

The cellulose-based fabric conveying unit 150 serves to convey the first cured cellulose-based fabric from the first curing agent injection unit 140 by a plurality of upper and lower rollers 151 and 152 zigzag installed up and down. .

The second curing agent injection unit 160 is located below the lower roller 152 of the cellulose-based fabric conveying unit 150 and the curing agent supplied from the curing agent supply unit 130 to the lower portion of the cellulose-based fabric to be transferred. Spraying serves to cure the cellulose-based fabric secondary.

The second curing agent injection unit 160 has the same structure as the first curing agent 140, and includes a curing agent inlet pipe 161 and an injection nozzle 162.

As described above, the present invention allows the curing agent to be adsorbed to the cellulose-based fabric by the second curing agent injection unit 160 to increase the fixing force of the flame retardant to increase the flame retardant property of the blended product. It can be improved.

The cellulose-based fabric discharge unit 170 serves to discharge the second cured cellulose-based fabric from the second curing agent injection unit 160 to the outside of the chamber 110.

The third curing agent injection unit 180 is provided below the cellulose-based fabric discharge unit 170 and the curing agent supply unit 130 to the lower portion of the cellulose-based fabric to be discharged by the cellulose-based fabric discharge unit 170 Spraying a curing agent supplied from the role of the third cure the cellulose-based fabric.

The third curing agent injection unit 180 has the same structure as the first curing agent injection unit 140 and the second curing agent injection unit 160, and the curing agent inlet pipe 181 and the injection nozzle ( 182).

As described above, the present invention allows the curing agent to be adsorbed to the cellulose fabric by the second curing agent cellulose fabric by the third curing agent injection unit 180 to increase the fixing force of the flame retardant to improve the flame retardant characteristics of the cellulose fabric. You can improve even more.

In addition, the present invention may be to be precipitated in the curing agent in order to give a soft touch and shrinkage property to the cellulose-based fabric. At this time, in order to give a soft touch and shrinkage property to the cellulose-based fabric, it is preferable to have a curing agent bath 191 and the bath lifting portion 192.

The cure agent bath 191 is provided between the first cure agent injection unit 140 and the cellulose-based fabric transfer unit 150, the cellulose primarily cured by the first cure agent injection unit 140 It serves to immerse the base fabric by the curing agent.

In the case of providing a soft touch and shrinkage property to the cellulose-based fabric, the cellulose-based fabric is immersed in the curing agent bath 191, and in order not to pass through the curing agent bath 191 to impart flame retardancy to the cellulose-based fabric. .

To this end, the bath lifting unit 192, the cellulose-based fabric first cured by the first curing agent injection unit 140 so as to be spaced apart or immersed from the curing agent accommodated in the curing agent bath 191.

At this time, in order to give the cellulose-based fabric a flexible touch and shrinkage property by raising the curing agent bath 191 by the bath lifting unit 192, the cellulose-based fabric passes through the curing agent bath 191, As the cellulose-based fabric is transferred by the cellulose-based fabric conveying unit 150 in a wet state, the curing agent is adsorbed to the blended product by the second curing agent 160.

Since the curing agent is not dried when the curing agent is absorbed by the cotton product by the second curing agent injection unit 160 in a wet state of the cellulose-based fabric, the cellulose-based fabric may not maintain flatness. In order to maintain the flatness of the cellulose-based fabric, it is preferable that the pressing unit 200 is provided to press both sides of the cellulose-based fabric.

The pressing unit 200 serves to press the both sides of the secondary cured cellulose-based fabric from the second curing agent injection unit 160 to maintain the cellulose-based fabric flat state.

The pressing unit 200 for pressing both sides of the secondary cured cellulose-based fabric is composed of a pressurizing drum 201, a pressurizing drum rotating part 204, a felt 202, and a felt rotating part 203. To lose.

The pressurized drum 201 is wound once so that one side of the second cured cotton product from the second curing agent spraying unit 160 is in contact with the outer circumference and wound by the second curing agent spraying unit 160. ) To the secondary cellulose-based fabric to the cellulose-based fabric discharge unit 170.

The pressurized drum rotating part 204 serves to rotate the pressurized drum 201.

The pressurized drum rotating part 204 includes a drive pulley 204a provided on a shaft of a drive motor (not shown) and a driven pulley 204c provided on a rotating shaft 204b provided at the center of the pressurized drum 201. And, the drive pulley 204a and the driven pulley 204c is connected to the transmission belt 204d for transmitting power.

The felt 202 is installed in contact with the outer periphery of the pressure drum 201 and the other side of the cellulose-based fabric secondary cured from the second curing agent injection unit 160 and the pressure drum 201 It is pressurized together and made into an endless track.

The felt rotating part 203 serves to rotate the felt 202 in an endless track. The felt rotating part 203 is to be provided with a felt rotating drum 203a for the felt 202 is wound around the felt 202 is rotated when the felt 202 is engaged with each other when the pressure drum 201 is rotated.

In addition, the cellulose-based fabric is preferably pressurized while heating the cellulose-based fabric to improve the flatness of the cellulose-based fabric while passing through the pressing unit 200.

To this end, it is preferable to supply steam to the pressurized drum 201 to pressurize while heating the secondary cured cellulose-based fabric from the second curing agent injection unit 160 by the pressurized drum 201. Do.

In addition, in order to recover the curing agent supplied into the chamber 110, the curing agent recovery pipe connected to the chamber 110 to recover the curing agent and the curing agent recovered to the curing agent recovery tube It is preferable to include a curing agent recovery portion to be recovered to the curing agent to be stored in the curing agent supply tank 131.

In addition, when the curing agent is supplied from the curing agent supply unit to the first curing agent injection unit, the second curing agent injection unit, and the third curing agent injection unit, the supply pressure may be 0.50 to 1.20 MPa, preferably 0.95 to 1.0 Mpa. . In this case, if the supply pressure is not appropriate, there may be a problem that crosslinking does not occur between the amine-based compound of THPC-UREA and the curing agent, and if it exceeds 1.20 Mpa, there may be a problem in processing safety due to excessive curing agent.

And, when injecting the curing agent to the cellulosic fabric from the first curing agent injection unit, the second curing agent injection unit and the third curing agent injection unit, the injection pressure is preferably carried out under 0.5 ~ 1.0 Mpa, preferably the injection pressure It is recommended to carry out under 0.5 ~ 1,0 Mpa. At this time, when the injection pressure is less than 0.5 Mpa, the curing agent is not properly injected to the inside of the cellulose-based fabric, and thus crosslinking does not occur between THPC-UREA and the Aman compound, there may be a problem that the long-term flame resistance is inferior. If Mpa is exceeded, there may be a problem of unnecessarily high injection pressure.

In addition, the three-stage curing agent is an amine curing agent, and may include 70 to 90% by weight of the amine compound, 1 to 5% by weight of the primary alcohol, and the remaining amount of glyoxal resin, preferably, the amine compound 75 ˜85% by weight, primary alcohol 1.5-4.0% by weight and the balance of glyoxal resin. In this case, if the content of the amine compound is less than 70% by weight may not secure sufficient flame retardant effect, if the content of the amine compound exceeds 90% by weight may have problems in crosslinking and fabric penetration.

In addition, the primary alcohol may be mainly used alcohols harmless to the human body such as ethyl alcohol, and may be used at least one selected, if the primary alcohol content is less than 1% by weight, there may be a problem in the penetration phase, 5 weight If it exceeds%, there may be a problem in the curing phase due to overreaction with the crosslinking agent and the amine system.

The amine-based compound may include an amine, a penetrant, and a fixing agent including at least one selected from amines represented by the following Chemical Formulas 1 to 3. In addition, the amine compound is 1 to 5% by weight of the penetrant, 5 to 10% by weight of the fixing agent and the residual amount of the amine, preferably 2 to 4% by weight of the penetrant, 5.5 to 8% by weight of the fixing agent and the residual amount of It may comprise the amine. At this time, the same as the penetrant and the fixing agent of the padding liquid can be used.

[Formula 1]

NHR ¹ R ²

R ¹ and in Formula 1 R ² is the same as or different from each other, and is a hydrogen atom, a straight chain alkyl group of C5 to C14, a ground alkyl group of C5 to C14, or an alkylene group of C5 to C12, preferably R ¹ and R ² is the same as or different from each other, and is a hydrogen atom, a straight alkyl group of C8 to C13, or a ground alkyl group of C8 to C13, except that R ¹ and Except where both R ² are hydrogen atoms.

[Formula 2]

NHR ³ R ⁴

R ³ and in Formula 2 R ⁴ is the same as or different from each other, and is a hydrogen atom, a straight alkyl group of C14 to C18, a ground alkyl group of C14 to C18, or an alkylene group of C14 to C19, preferably R ³ and R ⁴ is the same as or different from each other, and is a hydrogen atom, a straight alkyl group of C15 to C18 or a crushed alkyl group of C15 to C18, provided that R ³ and Except when R ⁴ is all hydrogen.

[Formula 3]

NHR ⁵ R ⁶

R ⁵ of Formula 3 and R ⁶ is the same as or different from each other, and is a hydrogen atom, a straight alkyl group of C19 to C25, a ground alkyl group of C19 to C25, or an alkylene group of C20 to C25, and preferably a hydrogen atom, a straight alkyl group of C19 to C22, or C19-C22 is a ground alkyl group, provided that R ⁵ and Except when all R ⁶ are hydrogen atoms.

Next, the four-step oxidation treatment can be carried out by immersing the cured cellulose-based fabric in a H ₂ O ₂ aqueous solution of 5 vol% or less, preferably 2 to 5 vol% concentration for 30 to 50 seconds. have. In this case, when the H ₂ O ₂ concentration of the H ₂ O ₂ aqueous solution exceeds 5% by volume, there may be a problem that excessive oxidation reactions occur, such as embrittlement of the fabric.

Next, the water washing step 5 is the first rinse treatment of the cellulose-based fabric subjected to oxidation treatment with hot water at 85-95 ° C. for 1 to 2 minutes, followed by sufficient second washing with cold water, unreacted THPC-Urea (p) and impurities such as formaldehyde and hexamethylene tetramine produced by the addition reaction are completely removed.

Flame retardant fabric of the flame-treated fabric performed in step 5 may be formed in the cellulose-based fabric of the final compound as shown in FIG. At this time, the chemical formula of Figure 3 is an example for helping the understanding of the present invention, it is not intended to limit the scope of the present invention.

Next, the drying of the six stages is a tenter (Tenter, Ilsung Machinery Co., Korea) that can constantly discharge the washed cellulose-based fabric, hot air 1,500 ~ 2,000 rpm and 1 ~ 30 under 160 ~ 170 ℃ Drying may be performed at a rate of m / min, but drying may be performed such that an overfeed of the dried cellulose-based fabric is 11.5 to 12.5%.

Cellulose-based fabric of the present invention prepared by the flame-proof processing method described above can increase the tensile strength 8 ~ 70% than the cellulose-based fabric not cured, based on the KS K 0521 standard, when measuring the tensile strength, preferably Tensile strength may be increased by 20 to 70%, more preferably 25 to 68.5%, than the cellulose-based fabric that is not cured.

In addition, the cellulose-based fabric may be a limiting oxygen index (LOI) of 24 to 30, when measured according to ASTM D2863-91 standard, preferably LOI may be 25.5 ~ 29.

In addition, the cellulose-based fabric is measured in accordance with KS K ISO 1005-C06 standard, washing fastness may be 4 to 5.

Hereinafter, the present invention will be described in more detail based on Examples. However, the following examples should not be construed as limiting the scope of the present invention.

[ Example ]

Preparation  1-1: Padding  Produce

30% by weight of flame retardant including THPC-urea condensate having the specifications shown in Table 1, 3.0% by weight of glyoxal resin, 0.1% by weight of penetrant (Triton X-100), and the remaining amount of water were mixed and thoroughly mixed The solution was prepared.

Next, an aqueous sodium hydroxide solution was added to the mixed solution to adjust the pH to 5.5 to prepare a padding solution.

Flame Retardant Specifications - Tetrakis Hydroxymethyl Phosphonium Chloride-Urea Precondensate (THPC: urea = 2: 1 molar ratio) molecular _{structure: (HOCH 2) 3 PClCH 2} NHCONHCH 2 PCl (CH 2 OH) 3
Specific Gravity: 1.28 ~ 1.30 (25 ℃)
Active ingredient: 68%
Phosphorous Values: 10% P
-Net phosphorus content per solid: 14.7% (10.0% × 100/68)

Preparation  1-2 to 1-4 and Comparative Production Example  1-1 to 1-8: Padding  Produce

The padding liquid was prepared in the same manner as in Preparation Example 1-1, but the padding liquid was prepared by varying the flame retardant content as shown in Table 2 below.

division Flame Retardant Content Glyoxal resin Penetrant pH Preparation Example 1-1 30 wt% 3.0 wt% 0.1 wt% 5.5 Preparation Example 1-2 35 wt% 3.5 wt% 0.1 wt% 5.5 Preparation Example 1-3 40 wt% 4.0 wt% 0.1 wt% 5.5 Preparation Example 1-4 45 wt% 4.5 wt% 0.1 wt% 5.5 Comparative Preparation Example 1-1 27 wt% 2.7 wt% 0.1 wt% 5.5 Comparative Preparation Example 1-2 48 wt% 3.5 wt% 0.1 wt% 5.5 Comparative Preparation Example 1-3 35 wt% 3.5 wt% 0.1 wt% 6.2 Comparative Preparation Example 1-4 35 wt% 3.5 wt% 0.1 wt% 5.0 Comparative Preparation Example 1-5 35 wt% 3.5 wt% - 5.5 Comparative Preparation Example 1-6 35 wt% 3.5 wt% 0.8 wt% 5.5 Comparative Preparation Example 1-7 35 wt% 2.5 wt% 0.1 wt% 5.5 Comparative Preparation Example 1-8 35 wt% 5.0 wt% 0.1 wt% 5.5

Preparation  2-1: Amine Cure  Produce

An amine compound was prepared by mixing 90 wt% of the amine compound represented by Formula 1-1, 3 wt% of Triton X-100 as a penetrant, and 7 wt% of glyoxal resin as a fixing agent.

Next, an amine curing agent was prepared by mixing 80 wt% of the amine compound, 2.5 wt% of ethanol, which is a primary alcohol, and the remaining amount of glyoxal resin.

[Formula 1-1]

NHR ¹ R ²

In Formula 1-1, R ¹ is a hydrogen atom, R ² is a straight alkyl group of C12.

Preparation  2-2: Amine Cure  Produce

In the same manner as in Preparation Example 2-1 An amine curing agent was prepared, but an amine curing agent was prepared using an amine represented by the following Formula 2-1 instead of the amine represented by Formula 1-1.

[Formula 2-1]

NHR ³ R ⁴

R ³ in Formula 2-1 is a hydrogen atom, and R ⁴ is a straight alkyl group of C18.

Preparation  2-3: Amine Cure  Produce

In the same manner as in Preparation Example 2-1 An amine curing agent was prepared, but an amine curing agent was prepared using an amine represented by the following Formula 3-1 instead of the amine represented by Formula 1-1.

[Formula 3-1]

NHR ⁵ R ⁶

R ⁵ in Formula 3-1 is a hydrogen atom, and R ⁶ is a straight alkyl group of C20.

Preparation  2-4 to 2-5 and Comparative Preparation  2-1 to 2-5: Amine Cure  Produce

An amine curing agent was prepared in the same manner as in Preparation Example 2-1, but each of the amine curing agents having a composition and composition ratio as shown in Table 3 was prepared.

division An amine compound Primary alcohol Glyoxal
Suzy Amine Penetrant Fixative Amine Compounds in Curing Agents
content Preparation Example 2-1 90 wt% 3 wt% 7 wt% 80 wt% 2.5 wt% Remaining balance Preparation Example 2-2 90 wt% 3 wt% 7 wt% 87 wt% 2.5 wt% Remaining balance Preparation Example 2-3 90 wt% 3 wt% 7 wt% 87 wt% 2.5 wt% Remaining balance Preparation Example 2-4 90 wt% 3 wt% 7 wt% 87 wt% 2.5 wt% Remaining balance Preparation Example 2-5 90 wt% 3 wt% 7 wt% 73 wt% 2.5 wt% Remaining balance Comparative Preparation Example 2-1 90 wt% 3 wt% 7 wt% 92.5 wt% 2.5 wt% Remaining balance Comparative Preparation Example 2-2 90 wt% 3 wt% 7 wt% 66.5 wt% 2.5 wt% Remaining balance

Example  One : Flameproof  Manufacture of cotton fabric

A cellulose-based fabric (cotton fabric) having a cotton fiber of 100% by weight, a density of 190T, a weight of 300g / m², and a number of warp yarn 30's / weft 30's was prepared.

Next, after immersing the cellulose-based fabric for less than 1 minute at 22 ~ 23 ℃ padding liquid prepared in Preparation Example 1-1, using a padding Mangle (Mangle) through a 3kgf pressure, 2m / min speed Squeezing (Squeezing) was turned on and padded.

Next, different concentrations of THPC-urea penetrated to the outside in the micelles can be migrated by heat and hardened on the surface of the blended fabric, so that heat can be uniformly released from the padded cellulose fabric. A tenter (Tenter, Ilsung Machinery Co., Korea) was dried for 90 seconds at 145 ℃. At this time, the moisture content (wet pick up contents) measured based on Equation 1 of the cellulose-based fabric dried using a moisture meter was 20%.

[Equation 1]

Wet pick up,% = (Weight of blended product before drying-Weight of blended product after drying) ÷ Weight of blended product after drying × 100 (%)

Next, curing was performed by spraying the primary, secondary and tertiary curing agents onto the cellulosic fabric using the high speed curing device shown in a schematic side view in FIG. 2. At this time, the curing agent used the amine curing agent prepared in Preparation Example 2-1. The supply pressure was 0.97 MPa when the curing agent was supplied from the curing agent supply unit to the first curing agent injection unit, the second curing agent injection unit, and the third curing agent injection unit. The spraying pressure was 1 Mpa when the curing agent was sprayed onto the cellulosic fabric from the first curing agent injector, the second curing agent injector, and the third curing agent injector.

Next, an oxidation process was performed by immersing the high-speed curing cellulose-based fabric in an aqueous solution of 3% volume of H ₂ O ₂ for 34 to 35 seconds.

Next, the oxidized cellulose-based fabric was placed in hot water at 90 ° C., washed with water for 1 minute and 30 seconds, and then washed with cold water sufficiently to form unreacted THPC-urea (p) remaining on the surface and the form produced by the addition reaction. Impurities such as aldehyde and hexamethylene tetramine were completely removed.

Next, the washed cellulose-based fabric is dried by using a tenter (Tenter, Ilsung Machinery Co., Korea) that can release heat at hot air 1,800 RPM and 14 to 15 m / min at 167 to 168 ° C. Drying was performed so that the feed (over feed) was 12% to prepare a final flame-retardant cellulose-based fabric.

Example  2 to Example  3 and Comparative example  1 to 2

To prepare a flame-retardant cellulose-based fabric (cotton fabric) in the same manner as in Example 1, but after the padding treatment, when the drying process, the moisture content of the cellulose-based fabric so that the moisture content (wet pick up) as shown in Table 3 below After drying, a high speed curing process, an oxidation treatment process, a water washing process, and a drying process were performed in the same manner as in Example 1.

Experimental Example  1: Measurement of the marginal oxygen index

The limit oxygen index of each of the flame retardant blended fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 2 was measured, and the results are shown in Table 4 below.

At this time, the limit oxygen index was measured according to the ASTM D2863-91 standard using a limit oxygen index tester (SUGA Co., Japan).

division Moisture content (%, wet pick up contents) Limit Oxygen Index (LOI) Example 1 20% 30.5 Example 2 30% 28.5 Example 3 45% 28.0 Comparative Example 1 8% 22.8 Comparative Example 2 55% 24.1

Looking at the limiting oxygen index of Table 4, in Comparative Example 1, when compared with Example 1, there was a problem that the LOI value is greatly reduced, and in Comparative Example 2, when compared with Example 3, did not show a large difference . Therefore, it was confirmed that the moisture content is about 10 to 50%, preferably about 20 to 45%.

Example  4 to 8 and Comparative example  3 to 15

After performing the padding process by varying the padding liquid as shown in Table 5, after drying the padded cotton fabric in a moisture content of 30% as in Example 3, Using this, a flame retardant cotton fabric was manufactured by performing a high-speed curing process, an oxidation treatment process, a washing process, and a drying process in the same manner as in Example 1.

division Padding Curing agent Example 1 Preparation Example 1-1 Preparation Example 2-1 Example 4 Preparation Example 1-2 Preparation Example 2-1 Example 5 Preparation Example 1-3 Preparation Example 2-1 Example 6 Preparation Example 1-4 Preparation Example 2-1 Example 7 Preparation Example 1-1 Preparation Example 2-2 Example 8 Preparation Example 1-1 Preparation Example 2-3 Example 9 Preparation Example 1-1 Preparation Example 2-4 Example 10 Preparation Example 1-1 Preparation Example 2-5 Comparative Example 3 not used Preparation Example 2-1 Comparative Example 4 Comparative Preparation Example 1-1 Preparation Example 2-1 Comparative Example 5 Comparative Preparation Example 1-2 Preparation Example 2-1 Comparative Example 6 Comparative Preparation Example 1-3 Preparation Example 2-1 Comparative Example 7 Comparative Preparation Example 1-4 Preparation Example 2-1 Comparative Example 8 Comparative Preparation Example 1-5 Preparation Example 2-1 Comparative Example 9 Comparative Preparation Example 1-6 Preparation Example 2-1 Comparative Example 10 Comparative Preparation Example 1-7 Preparation Example 2-1 Comparative Example 11 Comparative Preparation Example 1-8 Preparation Example 2-1 Comparative Example 12 Preparation Example 1-1 Comparative Preparation Example 2-1 Comparative Example 13 Preparation Example 1-1 Comparative Preparation Example 2-2

Experimental Example  2 : Color fastness  Measure

The fastness of washing of the blend of each of the examples and comparative examples of Table 5 was measured, and the results are shown in Table 6 below.

At this time, the wash fastness was measured according to KS K ISO 105-C06 standard using a laundry tester (Launder Ometer Co., Korea).

division Padding  Flame retardant
content( % ) 10 times  Laundry
(washing cycles) 20 times  Laundry 50 washes Comparative Example 3 0 4-5 2-3 2-3 Example 1 30 4-5 4-5 4-5 Example 4 35 4-5 4-5 4-5 Example 5 40 4-5 4-5 4-5 Example 6 45 4-5 4-5 4-5 Example 7 30 4-5 4-5 4-5 Example 8 30 4-5 4-5 4-5 Example 9 30 4-5 4-5 4-5 Example 10 30 4-5 4-5 4-5 Comparative Example 4 27 4-5 4-5 4-5 Comparative Example 5 48 4-5 4-5 4-5 Comparative Example 6 35 3-4 3-4 3-4 Comparative Example 7 35 3-4 3-4 3-4 Comparative Example 8 35 3-4 3-4 3-4 Comparative Example 9 35 3-4 3-4 3-4 Comparative Example 10 35 4-5 4-5 4-5 Comparative Example 11 35 4-5 4-5 3-4 Comparative Example 12 30 4-5 4-5 3-4 Comparative Example 13 30 4-5 3-4 2-3

Looking at the wash fastness measurement results of Table 6, in Comparative Example 3, Example 1, Examples 4 to 6 and Comparative Examples 3 to 5, regardless of the flame retardant content in the padding solution, all showed excellent wash fastness, otitis There was no phenomenon. This is because cotton fabrics treated with THPC-urea flame retardant are treated with an amine curing agent so that the inherent properties of cotton fabrics are preserved as they are. Therefore, there is no deformation even if water is absorbed and no shrinkage occurs after washing. Cotton fabrics treated with THPC-urea flame retardant using the ring process are cross-linked with the amine compound in the curing agent as a catalyst to form an inert polymer, while the active polymer forms an inert polymer inside the cotton fabric, which is not affected by washing. It is judged that durability is not formed.

In addition, in the case of Comparative Example 6 using a padding liquid having a pH exceeding 6, the fastness is lowered, and in Comparative Example 7 using the padding liquid having a pH of less than 5.2, the blended fabric inner surface fibers are embrittled, resulting in low fastness. Showed.

And, in Comparative Example 8 using a padding liquid containing no penetrant, the fastness was low, and in Comparative Example 9 using a padding liquid containing more than 0.5% by weight of penetrant, the fastness was low. . In addition, in the case of Comparative Example 11 in which glyoxal resin was used in excess of 4.5% by weight, there was a problem in that the washing fastness was inferior from washing 50 times.

In addition, in the case of Comparative Example 12 in which the content of the amine compound in the curing agent exceeded 90% by weight, the long-term washing stability was lowered compared to the example, and the content of the amine compound in the curing agent was 70% by weight. In the case of the comparative example 13 used below, the wash fastness showed very bad result.

Experimental Example  3: for washing Flameproof  And long-term flameproof stability measurement

Examples 1, 4 to 8 and Comparative Examples 4 to 6 and Comparative Examples 8 to 15 to measure the long-term flame resistance degree according to the number of washing of the blended fabric, the results are shown in Table 7 ~ Table 9. Table 7 shows the results of 10 washes, Table 8 shows 20 washes, and Table 9 shows the results of 50 washes.

In this case, flame retardant was measured for the burnability according to the washing concentration of the flame retardant in accordance with KS K 0585 standard using a flame retardant tester (United State Testing Co., USA).

division
(10 times of washing) Padding  Flame retardant
content( % ) Afterglow time
( Afterflame  time, sec) Remaining time
(Afterglow time, sec) Carbonization distance
(Char Length, cm) Comparative Example 3 0 36 45 30 Example 1 30 16 3 24 Example 4 35 6 0 18 Example 5 40 5 0 12 Example 6 45 0 0 9 Example 7 30 14 One 17 Example 8 30 13 One 16 Example 9 30 10 0 13 Example 10 30 12 One 14 Comparative Example 4 27 20 4 28 Comparative Example 5 48 5 0 12 Comparative Example 6 35 10 3 25 Comparative Example 8 35 27 36 25 Comparative Example 9 35 5 0 18 Comparative Example 10 35 22 31 26 Comparative Example 11 35 6 0 17 Comparative Example 12 30 15 2 15 Comparative Example 13 30 18 3 19

division
(20 times of washing) Padding  Flame retardant
content( % ) Afterglow time
( Afterflame  time, sec) Remaining time
(Afterglow time, sec) Carbonization distance
(Char Length, cm) Comparative Example 3 0 35 28 30 Example 1 30 17 0 25 Example 4 35 One 0 10 Example 5 40 One 0 8 Example 6 45 45 0 7 Example 7 30 15 One 19 Example 8 30 21 2 20 Example 9 30 14 0 20 Example 10 30 19 One 28 Comparative Example 4 27 20 4 28 Comparative Example 5 48 5 0 12 Comparative Example 6 35 13 5 26 Comparative Example 8 35 29 39 27 Comparative Example 9 35 12 3 26 Comparative Example 10 35 24 32 26 Comparative Example 11 35 7 2 16 Comparative Example 12 30 15 0 19 Comparative Example 13 30 25 9 33

division
(50 times of washing) Padding  Flame retardant
content( % ) Afterglow time
( Afterflame  time, sec) Remaining time
(Afterglow time, sec) Carbonization distance
(Char Length, cm) Comparative Example 3 0 35 35 30 Example 1 30 21 0 28 Example 4 35 5 0 15 Example 5 40 2 0 10 Example 6 45 0 0 8 Example 7 30 18 One 20 Example 8 30 23 2 32 Comparative Example 4 27 20 4 28 Comparative Example 5 48 5 0 12 Comparative Example 6 35 15 8 28 Comparative Example 8 35 32 41 28 Comparative Example 9 35 4 0 15 Comparative Example 10 35 26 34 28 Comparative Example 11 35 16 7 19 Comparative Example 12 30 26 24 24 Comparative Example 13 30 30 33 29

Looking at the Tables 7 to 9, in the case of Examples 1, 4 to 8, overall excellent flame resistance and long-term flameproof stability was obtained. In particular, when comparing Example 1 and Examples 4 to 6, when the flame retardant content in the padding liquid is 35% by weight or more, the flame resistance and long-term flame resistance stability was greatly improved. THPC-urea flame retardant-treated cotton fabrics using the curing process, while the active polymer forms an inert polymer through crosslinking with an amine compound as a catalyst, giving high durability combustibility to the fibrillated layer inside the cotton fabric. In addition, the flammability, residual time, and carbonization distance of cotton fabrics treated with THPC-urea flame retardant even after 50 times of repeated washings did not significantly affect the blended fabric regardless of the number of washing times.

However, in the case of Comparative Example 4 compared with Example 1, the flame resistance was greatly reduced, and in Comparative Example 5 compared with Example 5, there was almost no difference in the effect of improving flame resistance.

In addition, in the case of Comparative Example 6 using the padding liquid having a pH of more than 6, the padding treatment was not good, the flame retardancy was poor as the number of washing increases. And, in Comparative Example 8 using the padding liquid containing no penetrant, it showed very low flameproof and long-term flameproof stability as in Comparative Example 3, Comparative Example 9 using a padding liquid content of more than 0.5% by weight of the penetrant In the case, there was no significant difference from Example 4.

In addition, in the case of Comparative Example 10 using less than 3.0% by weight glyoxal resin, the flame resistance was not good, and in Comparative Example 11 using more than 4.5% by weight of glyoxal resin, the initial flame resistance is excellent, but washing As the number of times increased, there was a problem that the long-term flame retardant stability dropped sharply.

In addition, in the case of Comparative Example 12, the flame retardancy was excellent up to 20 times, but the long-term flame resistance was sharply decreased from 50 times, and in Comparative Example 13, the long-term flame resistance was sharply decreased from 20 times. Showed.

Experimental Example  4: limit oxygen index measurement and Color difference  Measure

(1) Limit oxygen index measurement

The limiting oxygen index of the flame retardant blended fabric that was washed 50 times in the same manner as in Example 2 was measured, and the results are shown in Table 10 below.

At this time, the limit oxygen index was measured according to the ASTM D2863-91 standard using a limit oxygen index tester (SUGA Co., Japan).

(2) color difference measurement

The color difference of the flame retardant blended fabric was washed 50 times in the same manner as in Example 2, the results are shown in Table 10 below. And the color difference is measured based on the comparative example 3.

Using a color difference meter (Macbeth Co., USA), the color difference (ΔE) for each treatment concentration of the flame retardant was measured based on the D65 light source and 10 viewing conditions.

division
(50 times of washing) Padding  Flame retardant
content( % ) Marginal oxygen index
( LOI ) Color difference
(E) Comparative Example 3 0 18.4 - Example 1 30 24.3 0.93 Example 4 35 26.0 0.97 Example 5 40 26.6 0.97 Example 6 45 28.1 0.93 Example 9 30 25.1 1.1 Example 10 30 24.5 0.95 Comparative Example 4 27 19.7 0.94 Comparative Example 5 48 28.2 1.03 Comparative Example 10 35 21.8 0.92 Comparative Example 11 35 26.3 1.08

Looking at the measurement results of Table 10, in Example 1, Examples 4 to 6, it can be seen that the LOI value was 24 or more, and has a low color difference value of less than 1.0.

On the contrary, in the case of Comparative Example 4, the LOI value was less than 20, and in the case of Comparative Example 10, there was a problem in that the LOI value was significantly lower than in Example 4. In addition, in Comparative Example 5 and Comparative Example 11, when compared with Example 6, there was no difference in the LOI value, but rather the color difference value exceeded 1.0.

Experimental Example  5: tensile strength measurement

Tensile strength of the flame retardant blended fabric was washed 50 times in the same manner as in Example 2, the results are shown in Table 11.

At this time, the tensile strength was measured according to KS K 0521 standard.

division
(50 times of washing) Padding  Flame retardant
content( % ) The tensile strength
( Mpa ) The tensile strength
% Increase ^{One )} Comparative Example 3 0 473.5 0% Example 1 30 512.8 8.29% Example 4 35 593.5 25.33% Example 5 40 675.8 42.72% Example 6 45 796.6 68.22% Example 9 30 521.2 8.54% Example 10 30 530.8 8.75% Comparative Example 4 27 495.7 4.68% Comparative Example 5 48 797.5 68.41% 1) Tensile strength increase rate (%) The increase rate is calculated based on the tensile strength value of Comparative Example 3.

Looking at the tensile strength measurement results of Table 11, in the case of Example 1, Examples 4 to 6, it can be seen that the tensile strength is significantly improved compared to Comparative Example 3 without using a flame retardant. However, in Comparative Example 4, compared with Example 1, the tensile strength increase rate was very low, and in Comparative Example 5, compared with Example 6, the tensile strength increase rate was very poor.

In general, when the flame retardant treatment of cotton fabric, the conventional flame retardant treatment method causes a decrease in the strength of the cotton fabric, while if the flame retardant treatment of the cotton fabric by the method of the present invention is THPC-urea flame retardant uniform to the center of the cotton fabric The high durability and flame retardancy is uniformly formed on the fibrillated layer of the cotton fabric, so that the tensile strength of the cotton fabric does not decrease due to THPC-urea flame retardant treatment. In addition, the tensile strength of the cotton fabric improved with each increase of the THPC-urea flame retardant, so the cotton fabric treated with the THPC-urea flame retardant was inactivated by crosslinking the amine compound in the amine curing agent with a catalyst. It is believed that the tensile strength is increased whenever the amount of flame retardant increases by forming an insoluble polymer of the film inside the cotton fabric while forming the polymer.

Although the embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above embodiments, but may be manufactured in various forms, and having ordinary skill in the art to which the present invention pertains. It will be understood by those skilled in the art that the present invention can be embodied in other specific forms without changing to the spirit or essential features of the invention. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive.

110: chamber 120: cellulose-based fabric inlet
130: curing agent supply unit 131: curing agent supply tank
132: vaporization equipment 133: curing agent storage tank
134: curing agent supply pipe 140: first curing agent injection portion
141, 161, 181: Curing agent inlet pipe 142, 162, 182: Injection nozzle
150: cellulose-based fabric transfer unit 151, 152: upper and lower rollers
160: second curing agent injection unit 170: cellulose-based fabric discharge unit
180: third curing agent injection unit 191: liquid curing agent bath
192: Beth lifting portion 200: Pressurizing portion
201: Pressurized drum 202: Felt
203: felt rotating part

Claims (12)

delete delete delete delete delete delete delete delete delete Flame retarding the cellulose-based fabric, or the cellulose-based fabric including the cellulose-based fiber and the regenerated rayon fiber, and then padding the fabric;
Performing a drying process by tentering the padded fabric for 60 seconds to 120 seconds at 130 to 150 ° C. to prepare a dried fabric having a wet pick up content of 30 to 45%;
Using a high-speed curing device, three steps of curing by spraying the amine curing agent with the amine curing agent to the dried cellulose-based fabric by curing;
Oxidizing the treated fabric by immersing it in an aqueous solution of H ₂ O _{2 at a} concentration of 2 to 5% by volume for 30 to 50 seconds;
5 steps of washing the oxidized fabric with water at 85 to 95 ° C. for 1 to 2 minutes and then washing with cold water for 2 times; And
The washed fabric is dried by hot air at a speed of 1,500 to 2,000 rpm and 1 to 30 m / min under 165 to 180 ° C., but the over cellulose is dried so that the over feed of the dried cellulose-based fabric is 11.5 to 12.5%. Performing a process including;
The cellulosic fibers include one or more selected from cotton, linen, hemp, and ramie,
The cellulose-based fabric includes a knit or woven fabric, the cellulose-based fabric has a cotton content of 50% to 100%,
In the first step padding treatment, the cellulosic fabric is immersed in a padding liquid of pH 5.2 to 6, and then padded with mangling squeezing at a pressure of 2.5 to 3.5 kgf and a speed of 1.0 to 30.0 m / min. Treatment and spraying at a pressure of 0,1 to 1.5 kgf,
The padding solution contains 30 to 45% by weight of flame retardant including Tetrakis Hydroxymethyl Phoshonium Chloride (THPC) -urea condensate, 3.0 to 4.5% by weight of glyoxal resin, 0.05 to 0.5% by weight of penetrant, and the balance of water. ,
The amine curing agent includes 70 to 90% by weight of the amine compound, 1 to 5% by weight of the primary alcohol and the remaining amount of glyoxal resin, wherein the amine compound includes an amine represented by the following Formula 1, High speed curing device
chamber;
A cellulose-based fabric inlet for introducing a cellulose-based fabric into the chamber;
Curing agent supply unit for supplying an amine curing agent;
It is provided on one side inside the chamber adjacent to the cellulose-based fabric inlet and the cellulose-based by spraying the amine-based curing agent supplied from the curing agent supply to the cellulose-based fabric introduced by the cellulose-based fabric inlet A first curing agent spraying unit configured to cure the primary fabric;
Cellulose-based fabric conveying unit for transferring the first cured cellulose-based fabric from the first curing agent injection portion by a plurality of upper and lower rollers zigzag up and down;
A second curing agent injection unit which is positioned below the lower roller of the cellulose-based fabric transfer unit and sprays the amine-based curing agent supplied from the curing agent supply unit to the lower portion of the cellulose-based fabric to be transported to cure the cellulose-based fabric secondaryly. ;
Cellulose-based fabric discharge unit for discharging the secondary cured cellulose-based fabric from the second curing agent injection unit to the outside of the chamber; And
A third is provided below the cellulose-based fabric discharge unit to spray the curing agent supplied from the curing agent supply unit to the lower portion of the cellulose-based fabric to be discharged by the cellulose-based fabric discharge unit to cure the cellulose-based fabric third It includes a curing agent injection portion;
When the amine curing agent is supplied from the curing agent supply unit to the first curing agent injection unit, the second curing agent injection unit, and the third curing agent injection unit, the supply pressure is 0.50 to 1.0 MPa,
When spraying the amine-based curing agent to the cellulose fabric from the first curing agent injection unit, the second curing agent injection unit and the third curing agent injection unit, the spray injection pressure is carried out under 0.5 ~ 1.0 Mpa,
The dried cellulose-based fabric of step 6 has a tensile strength increased by 8 to 70% compared to the cellulose-based fabric that is not cured when measured for tensile strength according to KS K 0521 standard,
The dried cellulose-based fabric of step 6 has a limiting oxygen index of 24 to 30 when measured according to ASTM D2863-91 standard, and laundry fastness when measured according to KS K ISO 1005-C06 standard. Flameproof processing method of the cellulose-based fabric, characterized in that the 4 to 5 grade:
[Formula 1]
NHR ¹ R ²
Of formula 1 R ¹ and R ² is the same as or different from each other, and is a hydrogen atom, a straight alkyl group of C5 to C14, a ground alkyl group of C5 to C14, or an alkylene group of C5 to C12, except that R ¹ and Except when both R ² are hydrogen atoms. delete delete

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