KR101226164B1 - Method for producing the electrically nylon conductive fiber - Google Patents

Abstract

PURPOSE: A method for applying conductivity to a nylon fiber is provided to lower price, and to fabricate a large amount of conductive fibers(10-1,000kg/batch). CONSTITUTION: A method for applying conductivity to a nylon fiber comprises: a step of removing impurities attached on the nylon fiber; a step of treating the nylon fiber with a hydrochloric acid at 50-65 deg. C for 25-50 minutes; a step of neutralizing the nylon fiber with a caustic soda solution, washing and etching the surface of the nylon fiber; a step of adding non-ionic surfactant and heating at 35-80 deg. C for 120-200 minutes for modifying the nylon fiber; a step of adding copper compounds, a reducing agent, a stabilizing agent, a complex agent, a pH adjusting agent, and a sulfur compound and treating at 35-65 deg. C for 200-400 minutes; a step of applying conductivity to the nylon fiber with copper; and a step of dehydrating and drying. [Reference numerals] (A1) Refining; (A2) Removing emulsions and impurities; (B1) Etching the surface of a fiber; (C1) Modifying the fiber; (C2) Coupling agent; (C3) Anti-gelation agent; (C4) Hydrolysis promoter; (C5) Auxiliary agent; (D1) Applying conductivity; (D2) Applying conductivity to the fiber; (E1) Treatment with an emulsion; (E2) Treatment with a functional emulsion; (F1) Dehydrating/drying; (F2) Dehydrating; (F3) Drying

Description

METHOD FOR PRODUCING THE ELECTRICALLY NYLON CONDUCTIVE FIBER}

The present invention relates to a method of imparting conductivity by converting nylon (Cu), which is an insulator, to a nylon fiber using a chemical energy difference (chemical reduction method). More specifically, the nylon fiber is combined with a silane coupling agent. The present invention relates to a method for imparting conductivity of nylon fibers to impart conductivity by a chemical reduction method after fiber modification treatment to modify a copper ions with a reactive agent.

It is known that most synthetic fibers and some natural fibers are charged by static electricity due to friction between fibers or friction between fibers and skin. Such generation of static electricity causes a great problem not only in the wearing of the coating but also in the industrial field. Known.

Therefore, in order to solve the static electricity generation problem of the fiber, a method for treating the antistatic agent in the post-treatment process, or imparting conductivity to the fiber itself has been developed.

As a method for imparting conductivity to the fiber itself, a method of preparing a conductive acrylic fiber having excellent volume resistance by precipitating a conductive copper sulfide nanoparticle composition having excellent conductivity to an acrylic fiber having an acrylonitrile repeating unit has already been performed. Many have been devised and used.

On the other hand, unlike acrylic fibers, nylon fibers do not have a metal-encapsulating functional group on their own, so the method applied to acrylic fibers could not adsorb or coordinate copper sulfide nanoparticle compositions.

In order to overcome this problem, nylon fibers are first contacted with hydrogen sulfide, and the hydrogen sulfide-introduced fibers are wetted with a metal salt solution such as copper sulfate aqueous solution to form a metal sulfide such as copper sulfide on the fiber. A method of imparting electrical conductivity has been proposed. However, these and other existing methods are all very demanding, have a large amount of sediment during the work process, have a high risk of harmful substances, and have adverse effects on the work environment. The stability of copper deposits was low, and the durability and washing fastness were very low, and there was a problem in that the conductivity was easily lost when repeated use for a long time.

In addition, nylon has a high elasticity and is sensitive to heat, and thus it is a reality that problems such as dichroism and internal and external color difference are caused even in general cheese dyeing. Until recently, as a method of imparting conductivity to NYLON, an expensive noble metal palladium catalyst was used to treat textiles to shield electromagnetic waves. This method cannot be applied to cheese. (Refer to palladium chloride (PdCl2) 10g / l 150,000 won).

The present invention has been made to solve the above problems, an object of the present invention is to use a cheese dyeing machine, through the refining, etching, surface modification, conductivity provision, dehydration and drying step, the fiber + coupling agent + copper sulfide chemical The present invention provides a method for imparting conductivity of nylon fibers having physically strong bonding (adherence) and excellent conductivity.

The object of the present invention is not limited to the above-mentioned object, and other objects which are not mentioned will be clearly understood from the following description.

The present invention is to achieve the above object, the method of imparting conductivity of the nylon fiber according to a preferred embodiment of the present invention, the refining step of removing impurities attached to the nylon fiber; After treating the nylon fibers in an aqueous solution of hydrochloric acid at a temperature of 50 to 65 ° C. for 25 to 50 minutes, neutralizing with a caustic soda solution and washing with water to etch the surface of the nylon fibers; A modification step of modifying the nylon fiber by treating water for 120 to 200 minutes while gradually raising the temperature to 35 to 80 ° C by adding a silane coupling agent, an alcohol gelling agent, a hydrolysis catalyst, and an auxiliary agent using water as a solvent; Adding a copper (Cu) compound, a reducing agent, a stabilizer, a complexing agent and a PH adjusting agent, and a sulfur compound to treat 200 to 400 minutes at 35 to 65 ° C. to impart conductivity to the nylon fiber with copper; And dewatering and drying the nylon fibers to which the conductivity is imparted so as to have a water content of 25 to 35%, and drying by applying heat.

According to a preferred embodiment, a low foaming nonionic surfactant is used in the refining step.

According to a preferred embodiment, in the modification step, a nonionic surfactant is further included to increase the dispersing effect.

According to a preferred embodiment, in the reforming step, the anti-gelling agent for alcohols is methanol when the coupling agent is methoxy silanes and ethanol is used when the coupling agent is ethoxy silanes. Is at least one selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4), the auxiliary agent is isopropyl alcohol (IPA) is used.

According to a preferred embodiment, in the imparting conductivity, the silver nitrate further includes a durability enhancer selected from the group consisting of silver sulfate and silver chloride.

According to a preferred embodiment, after the conductivity imparting step, at least one functional oil selected from the group consisting of tactile improver, water repellent, oil repellent, brush raising agent, rust preventive agent, softening agent, antistatic agent, coating agent, and antioxidant It further comprises an emulsion treatment step of tanning nylon fibers using.

According to the method of imparting the conductivity of the nylon fiber of the present invention, the nylon filament in the cheese form, by an easy method, it is possible to mass-produce (10 ~ 1,000kg / Batch) the conductive fiber while lowering the cost. The development of conductive fibers using the excellent properties of nylon (NYLON) prevents electrical, mechanical, and electrical discharges caused by static electricity, and uses industrial materials, clothing, which utilize electromagnetic shielding, antibacterial, deodorization, and heat storage capabilities of copper. It is expected to be easy to apply to functional household goods.

According to the present invention, the surface of the nylon filament in the cheese state is chemically corroded to increase the surface area and to generate wrinkles, strings and irregularities. In addition, the chemical physical bonding strength is increased by using a fiber reforming coupling agent, auxiliaries, and additives, and copper sulfide is deposited by chemical reduction on the modified fiber, and then a functional emulsion is treated to heat (wet heat → dry heat). ) To allow the fiber + coupling agent + copper sulfide to be chemically and physically strongly bonded (close), thereby providing a conductive fiber using the excellent properties of nylon (NYLON).

1 is a flowchart of a method for imparting conductivity of nylon fibers according to a preferred embodiment of the present invention.

Hereinafter, with reference to the accompanying drawings, it will be described in more detail the method for imparting the conductivity of the nylon fiber of the present invention.

1 is a flowchart of a method for imparting conductivity of nylon fibers according to a preferred embodiment of the present invention.

The method for imparting conductivity of the nylon fiber of the present invention is basically a refining step for removing oil and impurities, an etching step for etching the surface of the nylon fiber, a coupling agent, an antigelling agent, a hydrolysis accelerator, and an additive to modify the nylon fiber. Nitriding step, imparting conductivity to impart conductivity to nylon fibers, and dehydration drying step.

The method for imparting conductivity of the nylon fiber of the present invention is preferably carried out using a cheese / Loose combined dyeing machine equipped with a static pressure device in terms of efficiency.

Simultaneously operate the solution circulation from In → Out and Out → In 3 to 10 minutes while maintaining 2.0kg / ㎠ pressure as water or air at the same time as operating in product production (refining ~ conductive imparting) process. .

First, it prevents deformation of the filament or yarn of the cheese. Since 2.0kg / ㎠ pressure is applied to the whole tainted material (nylon fiber), there is no deformation by the pump water pressure. (Pump pressure: 0.4 ~ 0.7kg / ㎠ is preferred). Excessive flow of the solution by the pump causes the dead layer to collapse.

Second, because the circulation of the solution is constant, the reaction occurs evenly, preventing accidents and improving quality.

Third, the common phenomenon, which is the disadvantage of centrifugal pumps (when the temperature is high, changes from liquid to gas to decrease the pump water pressure), the constant pressure increases the boiling point. Can produce

Fourth, the four floors are kept constant after the end of the process, making it easier to work as a post-process re-inder and increasing productivity.

Next, each step of the method for imparting conductivity of the nylon fiber of the present invention will be described in more detail.

First, a refining step is performed to remove impurities attached to nylon fibers. The refining step is to remove impurities attached to the nylon fibers. The refining step is a process of removing the impurities attached to the chloride (filament) and the impurities attached in the process of preparing and preparing the yarn, preferably a low-bubble nonionic surfactant is used. The use amount of the nonionic surfactant is 1 to 2 g / l, the temperature is 55 to 65 ° C, and the treatment time is 30 minutes.

For the refined nylon fiber, the etching step is performed to etch the nylon fiber surface.

Since the cross section of a general synthetic fiber is circular, and the surface is smooth and the bonding force (cohesion force) of the coupling agent is weakened, as in the present invention, when the surface of the nylon filament is corroded (etched) to form irregularities, the surface area becomes large and subsequent processes are performed. Anchor effect in the product state after rough. However, it should be noted that excessive etching may weaken the properties of the fiber, and insufficient etching may weaken the anchor effect. Nylon filament etching of the present invention is neutralized with a solution of caustic soda 0.005 ~ 0.020g / l after hydrochloric acid 30 ~ 70g / l, temperature (50 ~ 65 ℃), 25 ~ 50 minutes after treatment.

Next, a reforming step of modifying the nylon fiber was performed by adding water to the solvent, adding a silane coupling agent, an alcohol gelling inhibitor, a hydrolysis catalyst, and an adjuvant and treating the mixture for 120 to 200 minutes while gradually raising the temperature to 35 to 80 ° C. Rough Modification of nylon fibers is carried out to improve the binding force between the high molecular fiber (organic) and metal ions (inorganic).

 Coupling agents used in the nylon fiber modification treatment include silane coupling agents, titanium coupling agents, aluminum coupling agents, and zirconium coupling agents, but these may be used in combination of one or two types, but the nylon fibers of the present invention may be treated. It is preferable to use a silane coupling agent as a coupling agent to make. It is preferable to have functional groups, such as a vinyl group, an amino group, a mercapto group, and an imidazole group, in a molecule | numerator among a silane coupling agent, and it is aminopropyl triethoxy silane, aminoethylaminopropyl triethoxy silane, mercaptopropyl trimethoxy silane. Or mercaptopropyltriethoxy silane can be used. As for the usage-amount of a silane coupling agent, 5-40 g / l is preferable.

The antigelling agent is used to assist the dissolution of the coupling agent and to prevent gelation, and alcohol antigelling agents are preferably used. It is good to stir thoroughly, adding a coupling agent to alcohol-type antigelling agent gradually. 5-20 g / l of alcohol gelling inhibitor is used, methanol is used for methoxy silanes, and ethanol is used for ethoxy silanes, and it is preferable to prevent cross reaction.

In the present invention, it is economical to use water as the main solvent of the silane coupling agent.

The hydrolysis catalyst may be used by one or more selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4) to promote hydrolysis of the coupling agent. The reason why the hydrolysis catalyst is used is that the better the hydrolysis of the coupling agent, the smoother the work in the post process and the better the quality. On the other hand, when the solubility is poor, the distance between molecules of the coupling agent is close, and the self-condensation reaction easily occurs, which causes defects. The amount of the silane coupling agent hydrolysis catalyst used is about 0.0005 ~ 0.001 g / l. In general, the dissolution of the silane coupling agent is suitable for pH 3 ~ 5, which is weakly acidic, and the stability of the solution is guaranteed, but in other areas, it is easy to gel by condensation reaction, and when gelled, it functions properly as a coupling agent. Attention is needed because it becomes infeasible. PH 7-10 are suitable for the coupling agent which has an amino group as a functional group.

Auxiliaries are used to increase the bonding strength between the fibers and the inorganic material (Bonding) to improve the durability. When using a coupling agent which has a vinyl group as a silane coupling agent, mercaptopropyl trimethoxy silane, mercaptopropyl triethoxy silane, and a functional group, isopropyl alcohol (IPA) can be used as an adjuvant. The amount of isopropyl alcohol used as a supplement is 10 to 30 g / l.

Surfactants may optionally be used as additives in the fiber modification step, which may optionally be used to facilitate dispersion and solution circulation. The surfactant is preferably a nonionic surfactant, and the amount of use thereof is appropriate for the critical micelle concentration.

The dissolution order of the preparations in the reforming step is first circulated by adding acetic acid (hydrolysis catalyst) to 1/3 of the total amount of water used. Next, the gelling agent is added to a separate PE container, and the mixture is stirred for 5 minutes or more while gradually adding the silane coupling agent to the solution into which acetic acid is added. Add the auxiliary IPA. If necessary, add an additive, a nonionic surfactant, and circulate at 25 ~ 35 ℃ for 15 ~ 25 minutes. Equipped with refined filament carrier (nylon fiber), adjusted solution ratio 1: 15 ~ 1: 20, pH 3 ~ 5 to operate solution circulation pump to maintain constant pressure (2.0kg / ㎠), and solution is 3 ~ It alternately circulates into In → Out, Out → In at 10 minute intervals, and slowly raises the temperature to 35 ~ 80 ℃ to treat 120 ~ 200 minutes and washes with warm water and cold water to remove unreacted material.

Next, for the modified nylon fiber, copper (Cu) compound, reducing agent, stabilizer, complexing and PH adjusting agent, sulfur compound were added and treated at 35 to 65 ° C. for 200 to 400 minutes to impart conductivity to the nylon fiber with copper. It is subjected to a conductivity providing step. In other words, the modified fibers are given conductivity by chemical reduction (chemical energy difference).

Copper (Cu) is a copper ion source, cupric sulfate (CuSO4.5H2O), cupric nitrate [Cu (NO3) 2], cupric chloride (CuCl2H2O), copper acetate [Cu (CH3COO) 2] etc. can be used 1 type or 2 types. The amount of copper (Cu) compound is 10 to 30 g / l.

The reducing agent is hydroxylamine sulfate [(NH3OH) 2SO4], hydroxylamine hydrochloride (NH2OH.HCl), sodium citrate [(CH2COONa) 2.2H2O], hypophosphite (NaH2PO2), formaldehyde (HCHO), dimethylamineborane [( CH 3) 2 HNBH 3], sodium hypophosphate (NaH 2 PO 2), sodium thiosulfate (Na 2 S 2 O 3), and sodium borohydride (NaBH 4). The amount of reducing agent is 10-30 g / l.

The stabilizer prevents the rapid reaction of the solution when the conductivity is imparted to maintain a stable state so that the reaction proceeds evenly. That is, it serves to even out the particles of copper sulfide produced and to prevent the formation of precipitates of copper sulfide. The stabilizer is a cyanide compound, thiourea [(NH2) 2CS], disodium phosphate (Na2HPO4.12H2O), and the like. The amount is 10 to 40 g / l.

Complexing and pH adjusting agents use EDTA, citric acid (C6H10O8), tartaric acid (C4H6O6), carbonic acid (H2CO3), hydrochloric acid (HCl), sulfuric acid (H2SO4), acetic acid (CH3COOH) and the like. The use amount of complexing and pH adjusting agent is 10-20 g / l.

The sulfur (S) compound evenly disperses and adsorbs copper ions reacted with fibers with copper sulfide to have conductivity. Sodium adithionate (Na2S2O4), acidic sodium sulfite (Na2S2O5), sodium thiosulfate (Na2S2O3), rongarite (NaHSO2HCHO.2H2O), sodium hydrogen sulfite (NaHSO3), etc. can be used. Sulfur compound used is 10 ~ 30g / l.

Durability enhancers may optionally be used in the conductivity provision step. Durability enhancers may be used silver nitrate (AgNO3), silver sulfate (Ag2SO4), silver chloride (AgCl), the amount is 0.10 ~ 0.50g / l. Durability enhancers serve to enhance durability and corrosion resistance.

When explaining the dissolution sequence of the preparations in the step of imparting conductivity, after dissolving the preparations by sufficiently stirring at 25 to 35 ° C. for 20 to 30 minutes, a salt solution Carrier (nylon fiber) is mounted and the liquid ratio is 1:15 to 1:20. , adjust pH 2.5 ~ 4.0 to operate solution circulation pump to maintain constant pressure (2.0kg / ㎠), and solution circulate alternately In → Out, Out → In every 3 ~ 10 minutes to even out the reaction. Prevents abnormal reactions and produces excellent products. Conductivity treatment temperature is 200 ~ 400 minutes at 35 ~ 65 ℃.

In the present invention, the imparting conductivity to nylon fibers is a method of imparting conductivity by chemical reduction method (chemical energy difference), and a crosslinking in which a hydrolyzed Si-OH group of a polymer material (fiber) and a silane coupling agent is combined with a metal salt (copper salt) Fiber surface layers are formed in various forms such as bonding (chemical adsorption) and hydrogen bonding, and especially the uneven parts of the fiber surface formed by etching exhibit excellent adhesion through the anchor effect, improving physical strength, electrical properties, and durability. Will also be better.

Next, an emulsion treatment for tanning nylon fibers using at least one functional oil selected from the group consisting of a tactile improver, a water repellent, an oil repellent, a raising agent, a rust preventive agent, a softening agent, an antistatic agent, a coating agent, and an antioxidant. Use steps selectively. In order to retain the functions of seaweed, knitting, weaving, hand, raising, function protection, water repellency, oil repellency, and rust resistance by treating the nylon fiber which has undergone conductivity in the refining step according to the needs of consumers. Make sure you have the right amount of fat. Normal maintenance of product is 0.35 ~ 1.00 wt% and it is adjusted according to purpose of use.

Next, the dehydrated nylon fibers to which the conductivity is given are 25 to 35% of water content, and are subjected to a dehydration and drying step of drying by applying heat.

Dehydration can be done using a general centrifugal dehydrator or a cheese dehydrator with high pressure air. It should be noted that excessive dehydration lowers the oil content, and insufficient dehydration is a waste of energy due to the rise of oil content and delay in drying time, and should be tested in advance. The water content after dehydration is preferably 25 to 35%.

For drying, a general hot air dryer or a high pressure cheese dryer may be used. The high pressure cheese dryer is ideal for energy saving, ease of operation, and shortening of drying time. The high pressure cheese dryer uses the property that the heat energy increases in proportion to the density of the air. The hot air of about 5 to 6 atmospheres is passed through the cheese to remove moisture contained in the chlorine with a condenser and then passes through the hot air again. It is a device to dry the process repeatedly. Refer to the hygrometer attached to the equipment to check and manage the contaminants and to optimize the operation method to prevent energy waste.

Next, the specific example is given and the method to give electroconductivity to the nylon fiber by the chemical reduction method of this invention is described. However, the following examples are only preferred examples of the present invention, and the present invention is not limited by the following examples.

 Nylon 70D / 24F filaments were treated with 1.5 g / l of low-foaming nonionic surfactant at about 60 ° C. for 30 minutes in hot water to remove emulsions and impurities and washed with water. Etching was treated for 40 minutes at 50 g / l hydrochloric acid, about 60 ° C., and then neutralized with 0.01 g / l caustic solution and washed with water. Next, the fiber modification is a pressure ratio of 1:20, pH 3-5 solution containing γ-mercaptopropyl methoxysilane 20g / l, methanol 15g / l, acetic acid 0.001g / l, IPA 20g / l static pressure (2.0 kg / cm 2) maintenance, alternately circulated from In → Out, Out → In at intervals of about 10 minutes, and slowly heated to 80 ° C. at room temperature for 180 minutes and washed with warm water and cold water to remove unreacted material.

The modified nylon filament was converted to 20 g / l cupric sulfate as a copper compound, 20 g / l as sodium thiosulfate reducing agent, 10 g / l as acidic sodium sulfite as a sulfur compound, 15 g / l as complexing and pH adjuster, and phosphoric acid as stabilizer. After dissolving the drug solution containing 20 g / l of disodium by stirring at 30 ° C. for about 25 minutes, dissolve the carrier solution, and adjust the liquid ratio to 1: 15 ~ 1: 20, pH 2.5 ~ 4 to adjust the solution circulation pump. It operated and maintained static pressure (2.0kg / cm <2>) and cycled alternately from In to Out and Out to In at about 10-minute intervals. The treatment temperature was treated at about 60 ° C. for 240 minutes, and then washed with warm water and cold water to remove the reaction residue and dehydrated / dried the emulsion.

Analysis result-Adsorbed evenly with olive green color, Cu content 3.0%,

The specific resistance was good at 3.0 x 10 ^{& lt} ; -1 &gt;

In addition to the drug of Example 1 in the step of imparting conductivity, 0.2g / l of silver nitrate (AgNO3) was additionally used in the same manner as in Example 1.

Analysis result-Adsorbed evenly with olive green color, Cu content in fiber 3.0%.

Specific resistance of 2.9 × 10 ^- was superior to ¹ (Ω.㎝).

Nylon (3D 38mm) Staple was washed with hot water at 60 ℃ to remove the spinning oil and impurities. Etching was treated with hydrochloric acid at 50 g / l and 60 ° C. for 30 minutes and neutralized with 0.01 g / l caustic solution and washed with water. The fiber modification treatment was carried out at a bath ratio of 1:15 to 1:20 containing 20 g / l of aminopropyltriethoxy silane, 15 g / l of ethanol, 0.001 g / l of acetic acid, 15 g / l of IPA, and 0.2 g / l of nonionic surfactant. Maintain constant pressure (2.0kg / ㎠) at pH 7 ~ 10, circulate alternating with In → Out, Out → In at intervals of about 10 minutes, gradually raise the temperature to 80 ℃, process it 180 minutes, and wash with warm water and cold water. Unreacted reaction was removed.

20 g / l cupric chloride, 20 g / l of reducing agent sodium thiosulfate, 10 g / l of sodium hydrogen sulfite as a sulfur compound, 15 g / l of complexing and pH adjuster, 20 g / l of disodium phosphate as stabilizer After thoroughly dissolving the containing chemical solution at 30 ° C. for about 25 minutes, dissolve the chlorine carrier, and adjust the bath ratio 1: 15 ~ 1: 20, pH 2.5 ~ 4.0 to operate the solution circulation pump to operate the static pressure (2.0kg / Cm 2), and cycled alternately from In to Out and Out to In at 10 minute intervals. The treatment temperature was 240 minutes at 60 ° C and washed with hot water and cold water sufficiently to remove the reaction residue and tanned dehydration / drying.

Analysis result-Adsorbed evenly with olive green color, Cu content of fiber 2.8%.

Specific resistance of 3.8 × 10 ^- was superior to ¹ (Ω.㎝).

Comparative example  One

Nylon (3D 38mm) Staple was washed with hot water at 60 ℃ to remove the spinning oil and impurities. It is placed in an aqueous solution of liquid ratio 1:20 containing 50% by weight of Acrylonitrile (AN), 1.5-2.0% by weight of ammonium persulfate, 2.5-3.5% by weight of sodium bisulfite, and 0.2% by weight of nonionic surfactant based on the weight of nylon staple. The temperature was raised to room temperature and treated with Graft at 80 ° C. for 70 minutes. The nylon staple treated as above is sufficiently washed with unreacted material. Based on the weight of the graft treated nylon staple, 20% by weight cupric sulfate, 15% by weight sodium thiosulfate, 4% by weight sodium hydrogen sulfite, 20 g / L dibasic sodium phosphate, and 15 g / L citric acid 1:20, pH 3 ~ 4 in aqueous solution is gradually raised to room temperature and treated for 240 minutes at 65 ℃.

After completion of the conductive treatment, it is rinsed sufficiently, and tanned-dehydrated / dried. The thus obtained nylon staple was unevenly adsorbed copper sulfide, so that the color difference was large, and the specific resistance was 4.1 × 10 ⁰ (Ω.㎝) and the Cu content in the fiber was 2.0%.

Comparative example  2

Nylon 80D / 24F was washed with water containing a nonionic surfactant, and washed with water and dried. The dried nylon filament was pretreated with a neoalkoxy titanate coupling agent having a thiocarbonyl group at 100 ° C. for 60 minutes and washed with water.

20% by weight of cupric sulfate, 5% by weight of hydrosulfide, 3.2% by weight of anhydrous sodium sulfite, 11% by weight of ferrous lactate, and adjusted the pH to 3.5 with citric acid and sodium diphosphate. The mixture was gradually warmed up at 60 ° C. for 180 minutes, then sufficiently washed and dried at 70 ° C. to 80 ° C.

Analysis Result: Color (Olive Green), Cu content in fiber 2.6%.

Specific resistance: 4.8 × 10 ^-1 (Ω.㎝)

Table 1 is a test result for the specific resistance and color change for Examples 1 to 3 and Comparative Examples 1 and 2.

division Resistivity (Ω.㎝) Color change Remarks Before the test After the test Before the test After the test Example 1 3.0 × 10 ^-1 3.1 × 10 ^-1 Olive green Olive green Slightly darker Example 2 2.9 × 10 ^-1 2.8 × 10 ^-1 Olive green Olive green Very weak dark color Example 3 3.8 × 10 ^-1 4.0 × 10 ^-1 Olive green Olive green Slightly darker Comparative Example 1 4.1 × 10 7.5 × 10⁴ Poor color decolorization Badly discolored Comparative Example 2 4.8 × 10 ^-1 5.5 × 10 Olive green Olive green Discolor to dark

 Specific resistance test conditions: temperature (20 ± 2 ℃), humidity (40 ± 2%),

                  Test Equipment-WHEATSTONE BRIDGE (Fortable)

 Durability test conditions: relative humidity (RH 100%), temperature (60 ℃), time (100Hr.)

                  Test Equipment-Automatic Thermo-hygrostat

Referring to Table 1, Examples 1, 2 and 3 showed a very excellent effect compared to Comparative Examples 1 and 2. The second embodiment is because the bonding stability of the copper sulfide is improved by using silver nitrate as the durability enhancer, thereby improving the corrosion resistance. On the other hand, in Comparative Example 1, it was difficult to remove non-uniform reactants and non-uniformity of the condensation reaction using AN, and the color and performance durability significantly differed after the conductive treatment. Comparative Example 2 is better than the AN condensation reaction method, but the binding strength of the silane coupling agent is weak, and color change (oxidation) is easily observed. This is because the bond strength between the fiber and the coupling agent copper sulfide is weak, so that the surface of the fiber is damaged even with a weak external force, so that the copper sulfide is easily peeled off and oxidized.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. It will be appreciated that various changes and modifications may be made therein without departing from the scope of the invention.

Claims (6)

Refining step of removing impurities attached to the nylon fiber;
After treating the nylon fibers in an aqueous solution of hydrochloric acid at a temperature of 50 to 65 ° C. for 25 to 50 minutes, neutralizing with a caustic soda solution and washing with water to etch the surface of the nylon fibers;
Water is used as a solvent, and a silane coupling agent, an alcohol gelling agent, a hydrolysis catalyst, an auxiliary agent, and a nonionic surfactant for increasing the dispersing effect are added, and the mixture is treated at 120 to 200 minutes while gradually warming to 35 to 80 ° C. A modification step of modifying the nylon fibers;
Adding a copper (Cu) compound, a reducing agent, a stabilizer, a complexing agent and a PH adjusting agent, and a sulfur compound to treat 200 to 400 minutes at 35 to 65 ° C. to impart conductivity to the nylon fiber with copper; And
The dehydration and drying step of dewatering the nylon fibers to which the conductivity is imparted so as to have a water content of 25 to 35%, and drying by applying heat. The method of claim 1,
The method for imparting conductivity of nylon fibers, characterized in that a low-bubble nonionic surfactant is used in the refining step. delete The method of claim 1,
In the modification step,
Alcohol-gelling inhibitors include methanol when the coupling agent is methoxy silanes and ethanol when the coupling agent is ethoxy silanes.
The hydrolysis catalyst is one or more selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4),
The auxiliary agent is a method for imparting conductivity of nylon fibers, characterized in that isopropyl alcohol (IPA) is used. The method of claim 1,
In the conductivity provision step,
Silver nitrate, sulfuric acid, silver chloride and silver chloride further comprises a durability enhancer selected from the group consisting of a method for imparting conductivity of nylon fibers. The method of claim 1,
After the imparting conductivity,
Added an emulsion treatment step of tanning nylon fibers with a functional oil selected from at least one selected from the group consisting of tactile improvers, water repellents, oil repellents, brushing agents, antirust agents, softening agents, antistatic agents, coating agents, and antioxidants. Conductive imparting method of nylon fiber, characterized in that it comprises a.

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