KR101599029B1 - Composite non-woven fabric and process for preparing the same - Google Patents

Abstract

Disclosed are a composite non-woven fabric and a manufacturing method thereof, which comprises: a non-woven substrate composed of one or more selected from a group consisting of polylactic acid fiber, polycaprolactone fiber and lactic acid-glycolic acid copolymer fiber formed by electrospinning; and a coating layer of carboxylmethyl cellulose formed on at least one among both sides of the non-woven substrate or the inner pores of the non-woven substrate, wherein the composite non-woven fabric becomes opaque when not absorbing moisture and becomes transparent when absorbing moisture.

Description

[0001] Composite nonwoven fabric and process for preparing same [0002]

More particularly, the present invention relates to a composite nonwoven fabric having excellent liquid-absorbent properties and high transparency when absorbed, which is directly coated on a wound surface to serve as temporary artificial skin, and a method for producing the composite nonwoven fabric .

Skin is an important organ that occupies the largest surface area of our body, which protects the human body from various harmful environments such as external microorganisms, ultraviolet ray and chemical substances, to be.

On the other hand, as the industrial society develops, the possibility of skin damage due to various causes such as severe burns, trauma, wounds, pressure ulcers and skin diseases is increasing. At this time, wounds that can not be primaryly sealed are severely defective .

Therefore, restoration of damaged skin tissue is a very important problem. In order to accelerate the treatment of wounds and to minimize secondary side effects, wound treatment using appropriate wound dressings is essential.

In particular, the skin of a human body has a property of defending and naturally healing the wound area in case of wound, burn, etc. In this case, a wound dressing material is used as a method for effectively protecting the wound area and increasing the healing speed. The characteristics of the wound dressing should be such that it has excellent biocompatibility so that there is no rejection reaction to the wound area and it is enough to absorb the body fluids discharged from the wound area and has high moisture permeability to prevent normal skin burning around the wound And the ability to maintain breathability.

Conventional thin-film wound dressings promoted wound healing by promoting the dissolution of necrotic tissue and formation of granulation tissue by maintaining the wound area in a moist state. However, excessive amounts of body fluids such as body fluids around the wound are promoted, There is a problem that the skin is worn out and the discharged product leaks out, and the product should be discharged arbitrarily. In addition, there is a drawback in that pores must be additionally physically / chemically formed to improve the moisture permeability.

In addition, since the wound site was covered with the wound dressing, the wound healing process could not be observed, the healing process could not be checked, or the necessity of the wound infection or bandage replacement could not be checked, so the wound dressing had to be removed. In this case, even though the wound is not sufficiently healed, the wound dressing is removed, which can cause serious problems such as damage to the skin and obstruction of the healing process.

Therefore, there is a continuing need to develop a wound dressing material having both absorbency and transparency to the effluent at the wound site.

A problem to be solved by the present invention is to provide a composite nonwoven fabric having excellent liquid-absorbent properties and high transparency when absorbed, and which is directly coated on a wound surface to serve as temporary artificial skin.

Another problem to be solved by the present invention is to provide a method for producing the composite nonwoven fabric.

Another object to be solved by the present invention is to provide a sanitary article using the composite nonwoven fabric.

To solve these problems, according to one aspect of the present invention,

A nonwoven fabric substrate made of one or more fibers selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer formed by electrospinning; And

A carboxymethyl cellulose coating layer formed on at least one of the both surfaces of the nonwoven fabric substrate or the inner pores of the nonwoven fabric substrate,

A composite nonwoven fabric which is opaque in a non-absorbent state and transparent in a liquid absorbent state is provided.

The average pore size of the composite nonwoven fabric may be 5 탆 or less.

The fibers may have an average diameter of 100 to 4,000 nm.

The content of lactic acid in the lactic acid-glycolic acid copolymer may be 10 to 90 molar equivalents.

The loading amount of the carboxymethylcellulose coating layer may be 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric base material.

The transparency of the composite nonwoven fabric after being immersed in 0.9% physiological saline solution for 30 seconds may be 60% or more.

The absorption capacity of the composite nonwoven fabric may be 4 g / g or more.

According to another aspect of the present invention,

Preparing an electrospinning solution by dissolving one or more selected from the group consisting of polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymer in a solvent;

Forming a nonwoven fabric base by electrospunning the spinning liquid; And

And coating a carboxymethyl cellulose solution on the nonwoven fabric substrate to form a carboxymethylcellulose coating layer.

The carboxymethylcellulose solution can be prepared by dissolving carboxymethylcellulose in water and a mixed solvent of non-solvent of the carboxymethylcellulose and non-solvent having lower surface tension than water.

The content of the non-solvent in the mixed solvent may be 5 to 60% by weight.

The non-solvent of the carboxymethyl cellulose may be at least one selected from the group consisting of alcohol, acetone, methylene chloride, and chloroform.

The method may further include calendering the nonwoven fabric substrate before or after coating the carboxymethylcellulose solution after the electrospun to form the nonwoven fabric substrate.

According to another aspect of the present invention, there is provided a sanitary article using the above-described composite nonwoven fabric.

The sanitary article may be a medical covering, an absorbent sanitary article, a food packaging material, or a mask pack.

According to the present invention, there is provided a composite nonwoven fabric which has excellent liquid-absorbing properties and high transparency when absorbing liquid, acts as a temporary artificial skin directly coated on the wound surface, can prevent the infiltration of bacteria from external infectious agents, Thereby providing a sanitary article using the same.

BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate preferred embodiments of the invention and, together with the description of the invention given below, serve to further augment the technical spirit of the invention. And should not be construed as limiting.
1 is a graph showing the hydrophilicity of the composite nonwoven fabric prepared in Example 1 and the nonwoven fabric prepared in Comparative Example 1.
2 and 3 are photographs showing the results of evaluating the transparency of the composite nonwoven fabric prepared in Example 1 and the nonwoven fabric prepared in Comparative Example 1, respectively, upon absorption.
Fig. 4 is a photograph showing the results of comparative evaluation of the transparency of Example 1 and Comparative Example 3 in absorbing liquid.
5 and 6 are SEM photographs of the surfaces of the composite nonwoven fabric produced in Example 1 and Comparative Example 3, respectively.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be interpreted in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined.

Therefore, the embodiments described in the present specification and the configurations shown in the drawings are only the most preferred embodiments of the present invention and do not represent all the technical ideas of the present invention. Therefore, It is to be understood that equivalents and modifications are possible.

Polylactic acid (PLA) refers to the entire polymer composed of lactic acid as a monomer. It is a polymer chemically synthesized by using L-lactic acid, which is made by fermenting microorganism from renewable resources such as polymeric lactic acid and starch, as a monomer , Isomer D-lactide, and L-lactide content (random copolymerization, block copolymerization).

A lactic acid-glycolic acid copolymer (PLGA) is a copolymer having repeating units derived from polylactic acid and polyglycolic acid in common. At this time, the polyglycolic acid is an aliphatic polyester having a very simple structural unit (-O-CH ₂ -CO-) and has a property of being absorbed and decomposed in vivo.

As a result, such polylactic acid and lactic acid-glycolic acid copolymer are globally recognized biocompatible, biodegradable thermoplastic polyesters, and are generally widely used as medical products and biomaterials.

However, the polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer are wholly or partly hydrophobic or have a low degree of wettability. Therefore, when polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymer are used as a material for medical use, particularly wound dressing, the liquid absorbing properties of the secretion liquid discharged from the wound area are lowered to improve the adhesiveness to the wound site, There was a limit in that the function could not be sufficiently exhibited. Further, in order to prevent a second injury caused by an external infectious agent at the wound site, there is an increasing need to control the pore size of the tissue during the development of materials using the polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer. In addition to the improvement of the hygroscopicity, it is further demanded that the state of the wound site can be easily observed even when the wound site is coated, thereby enabling treatment and treatment to be performed in a timely manner.

In order to address the need for the latest and various properties of such medical materials, the present inventors have found that a nonwoven substrate made of fibers of polylactic acid, polycaprolactone or lactic acid-glycolic acid copolymer formed by electrospinning; And a carboxymethylcellulose coating layer formed on at least one of the both surfaces of the nonwoven fabric substrate or the inner pores of the nonwoven fabric substrate, wherein the composite nonwoven fabric is opaque in a non-absorbed state and transparentized in a liquid absorbed state.

The nonwoven fabric substrate of the composite nonwoven fabric is composed of one or more fibers selected from the group consisting of polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymer formed by electrospinning.

As described above, the polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer provide superior biocompatibility and biodegradability, which are basically required characteristics of the present composite nonwoven fabric.

At this time, the content of lactic acid in the lactic acid-glycolic acid copolymer may be adjusted to preferably 10 to 90 molar equivalents, more preferably 10 to 70 molar equivalents. In the case of controlling the content of lactic acid, the solution for electrospinning is easy to produce, the biodegradability is improved, and even if it remains on the wound surface, biodegradation may occur with time.

In the present invention, the nonwoven fabric substrate is formed by electrospinning fibers. The nonwoven fabric substrate can be formed into a thin film by sufficiently exhibiting properties of biodegradable and biocompatible polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymer, It is possible to easily adjust the pore size of the base material, to have high flexibility, and to improve the covering property to the skin.

The fibers of lactic acid, polycaprolactone and lactic acid-glycolic acid copolymer forming the nonwoven substrate have an average diameter of 100 to 4,000 nm, more preferably 500 to 3,000 nm. When the diameter of the fiber satisfies this range, the pore size of the base material can be controlled to be sufficiently small and the flexibility of the nonwoven fabric can be improved without increasing the thickness of the nonwoven fabric base.

The composite nonwoven fabric according to the present invention comprises a carboxymethylcellulose coating layer on at least one of the both surfaces of the nonwoven substrate or the inner pores of the nonwoven substrate.

The carboxymethyl cellulose coating layer improves the disadvantages of the hydrophobic property of the nonwoven fabric base made of one or more kinds of fibers selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer to improve hydrophilicity, And maintains the wet environment in the wound area. Also,

The loading amount of the carboxymethylcellulose coating layer may be 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric base material. When the loading amount of the carboxymethyl cellulose coating layer satisfies this range, it is possible to improve the absorption characteristics of the final composite nonwoven fabric and to easily control pores so as to prevent invasion of bacteria from an external infectious source.

The carboxymethylcellulose coating layer may be coated on at least one surface of the nonwoven fabric substrate, or the coating layer may be formed by incorporating carboxymethylcellulose into the space inside the pores according to the pore size control of the nonwoven fabric substrate. Particularly, the greater the degree to which the carboxymethyl cellulose coating layer is embedded in the space inside the pores of the nonwoven fabric substrate, the better the liquid absorbing properties as well as the surface of the nonwoven fabric substrate surface, and the overall liquid absorbing capacity of the nonwoven fabric substrate can be increased. As a result, when the composite nonwoven fabric of the present invention is applied to a wound site, the absorption characteristics with respect to a secretion liquid such as body fluids and the like can be remarkably improved, resulting in better results in wound healing.

The average pore size of the composite nonwoven fabric may be 5 μm or less, preferably 0.2 to 5 μm, more preferably 0.5 to 2 μm. The average pore size of the composite nonwoven fabric may be affected depending on the average size of the nonwoven fabric base initially, the loading amount of the coated carboxymethylcellulose coating layer, and the coating pattern. If the calendering process is performed after forming the carboxymethylcellulose coating layer on the nonwoven fabric substrate, the average pore size of the composite nonwoven fabric can be controlled according to the conditions of the calendering process, that is, the temperature and the pressure.

When the average pore size of the composite nonwoven fabric satisfies the above range, an external infectious agent such as Staphylococcus aureus can be prevented from approaching the wound site through the composite nonwoven fabric, and adequate ventilation can be imparted.

The composite nonwoven fabric may include a carboxymethylcellulose coating layer on a nonwoven fabric substrate made of one or more fibers selected from hydrophobic polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer, And is improved. The liquid-absorbent properties of the composite nonwoven fabric can be evaluated by changing the weight before and after the liquid-absorbing in a sample of a predetermined weight, as described below.

Absorbing magnification (g / g) = [(weight of sample after liquid absorption) - (weight of sample before liquid absorption)] / (weight of sample before liquid absorption g)

The absorption capacity of the composite nonwoven fabric may be 4 g / g or more, preferably 4 to 30 g / g, and more preferably 6 to 20 g / g. When the liquid-absorbing power of the composite nonwoven fabric satisfies this range, the wound site is placed in a proper wetting environment when the wound area is coated, and the skin adhesion of the nonwoven fabric can be improved by absorbing the body fluid discharged from the wound area.

The composite nonwoven fabric according to the present invention is opaque in the non-liquid-absorbing state and has transparency in the liquid-absorbing state. This property is attributed to the fact that the skin adhesion of the nonwoven fabric is improved and the light scattering property is decreased with the absorption.

In general, if you are injured in your skin, it is important to look at the process of wound healing in order to be able to handle it properly. However, since the state of the wound surface of a normal nonwoven fabric is not visible, it is troublesome to observe the skin condition after removing the wound dressing made of nonwoven fabric in order to observe the wound area. At this time, Removal of the wound dressing can cause severe pain to the patient.

In this connection, the transparency of the composite nonwoven fabric after being immersed in 0.9% physiological saline solution for 30 seconds may be 60% or more, preferably 60 to 95%, more preferably 75 to 90%. Transparency was measured using a Gretag Macbeth colorimeter (CE 3100) using the reflectance measurement method at 400 to 700 nm under the visible light wavelength range under a D65 standard light source according to the following equation.

O _p = 100 -? R _i / j

O _p : transparency (%)

Reflectance corresponding to R _i = i ( i = 1 to j ) th wavelength value

j = number of reflectance measurement times

When the transparency of the composite nonwoven fabric satisfies this range, it is easy to observe the wound site even when the composite nonwoven fabric is adhered to the composite nonwoven fabric when the body fluid or the physiological saline solution is absorbed into the composite nonwoven fabric.

Further, when the composite nonwoven fabric is in a non-absorbent state, it is opaque means that the transparency is less than 60%.

The composite nonwoven fabric of the present invention may have a thickness of 50 to 500 mu m, more preferably 100 to 300 mu m. When the thickness range of the composite nonwoven fabric is satisfied, it is advantageous to improve transparency and flexibility of the nonwoven fabric.

Another aspect of the present invention provides a method for producing a composite nonwoven fabric, which comprises dissolving a mixture of one or more selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer in a solvent to prepare an electrospinning solution step; Forming a nonwoven fabric base by electrospunning the spinning liquid; And coating a carboxymethyl cellulose solution on the nonwoven fabric substrate to form a carboxymethylcellulose coating layer.

Electrospinning is used to prepare the nonwoven substrate of the present invention. For electrospinning, an electrospinning solution should be prepared by dissolving one or more compounds selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer in a solvent.

In order to prepare an electrospinning solution in the present invention, the solvent used may be a homogeneous solution of one or more of a mixture of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer, These higher solvents may be used without limitation, examples of which include trifluoroacetic acid, dimethyl formamide, dimethyl sulfoxide, chloroform, trifluoroethylene, acetone, hexafluoroisopropanol, methylene chloride, tetrahydrofuran, acetic acid and formic acid Etc. may be used, and these may be used as one or two or more mixed solvents.

At this time, the content of one or more mixture selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer added in the electrospinning solution is preferably 5 to 20 wt% By weight to 8-15% by weight. When the weight% is controlled, it is possible to obtain an electrospinning solution which is uniformly dissolved and has an appropriate viscosity and is easy to handle, and as a result, the spinning property can be improved and the diameter distribution of the produced fiber can be made uniform.

Preferably, a mixture of one or more compounds selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer is used as a co-solvent of dimethylformamide and chloroform excellent in radioactivity and easy to remove residual solvent Can be completely dissolved so as to be free from impurities, stirred for about 12 hours at room temperature, and then used for electrospinning.

Next, the prepared electrospinning solution is electrospun to form a nonwoven substrate.

According to the conventional electrospinning system and theory, the electrospinning process must be performed under a high voltage, and the air condition inside the chamber is also important because of the nature of electrostatic radiation. When the fiber is manufactured by the general process as described above, the shape of the fiber is slightly changed due to the characteristics of the electrostatic process sensitive to the environment (temperature, humidity) of the spinning chamber, and it is difficult to make a reproducible material.

In particular, polymers such as polylactic acid, polycaprolactone, or lactic acid-glycolic acid copolymer are not uniform in molecular weight due to their properties, and therefore control of process conditions in the production of fibers by electrospinning is important.

The basic electrospinning device used in the present invention is a syringe fitted with a 21G to 24G nozzle made of a stainless steel material in a unitary structure of a (+) charge high voltage generator, an accumulation drum and a constant-volume discharge pump. In the present invention, the structure and shape of each fiber sheet are determined according to the concentration of the solution, the applied voltage, the scattering range, the fluid velocity and the like which have important influence on the fiber shape among the various process factors and the electrospinning condition having the best reproducibility is obtained Respectively.

The electrospinning device according to an embodiment of the present invention may be an electrospinning solution prepared by dissolving one or more compounds selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer in a solvent Any apparatus capable of electrospinning can be applied without limitation, examples of which include syringe type, wire type, drum type, and the like, but are not limited thereto.

In the present invention, the electrospinning is preferably carried out under the conditions of electrospinning of a concentration of the mixed solution of 5 to 20% by weight, a voltage of 5 to 100 kV, a solution discharge rate of 0.1 to 10 ml / h and a radiation distance of 3 to 50 cm .

Next, a carboxymethylcellulose solution is coated on the obtained nonwoven substrate to form a carboxymethylcellulose coating layer.

The carboxymethylcellulose solution may be prepared by dissolving carboxymethylcellulose in a mixed solvent of water and alcohol.

Typically, carboxymethylcellulose is well soluble in water, whereas polylactic acid, polycaprolactone, or lactic acid-glycolic acid copolymer is hydrophobic, so it is preferable to use polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymer as an aqueous solution of carboxymethylcellulose It is difficult to uniformly adhere the aqueous solution of carboxymethylcellulose to the nonwoven fabric base material when coating the nonwoven fabric base material composed of one or more kinds of fibers selected from the group consisting of polyvinyl alcohol, However, when a non-solvent such as carboxymethyl cellulose is mixed as a solvent and a non-solvent having a surface tension lower than that of water is mixed with water, the surface tension of the obtained solution is less than that of the aqueous solution so that the carboxymethyl cellulose solution can be uniformly coated on the nonwoven substrate.

At this time, the content of the non-solvent in the mixed solvent is 5 to 60 wt%, more preferably 10 to 30 wt%. When the content of the non-solvent is less than 5%, the effect of adding the non-solvent is insignificant. When the content of the non-solvent is less than 60%, the non-soluble carboxymethyl cellulose does not dissolve and thus the carboxymethyl cellulose is insolubilized to precipitate or aggregate have.

As the non-solvent, alcohols such as methanol, ethanol and isopropyl alcohol, acetone, methylene chloride, chloroform, etc. may be used alone or as a mixture of two or more kinds.

At this time, when the carboxymethyl cellulose solution is coated on the nonwoven fabric substrate, the coating amount of the carboxymethylcellulose solution can be adjusted so that the loading amount of the carboxymethylcellulose coating layer is 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric base material have.

The nonwoven fabric base coated with the carboxymethylcellulose solution may be hot air dried or vacuum dried at room temperature or 40 to 120 ° C to obtain a composite nonwoven fabric.

Further, after the drying treatment, the obtained composite nonwoven fabric may be further subjected to a calendering process at a temperature of from room temperature to 100 DEG C at a pressure of 200 to 600 psi. By the calendering step, the pore size and thickness of the composite nonwoven fabric finally obtained can be controlled.

The composite nonwoven fabric of the present invention can be used for various medical coating materials, absorbent sanitary articles, food packaging materials, mask packs and the like, and may have particularly suitable characteristics as a wound dressing material serving as temporary artificial skin during burn treatment.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail with reference to the following examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the following embodiments. Embodiments of the invention are provided to more fully describe the present invention to those skilled in the art.

Example 1

An electrospinning solution was prepared by dissolving lactic acid-glycolic acid copolymer (PLGA) (lactic acid: glycolic acid = 70:30 by weight) in a mixed solvent of dimethylformamide (DMF) and chloroform (weight ratio = 1: 9) Prepared.

Thereafter, using a electrospinning device, the voltage was fixed at 15 kV, the radiation distance was 20 cm, and the fluid velocity was set to 6 ml / h, and the mixture was spin-coated on a rotating drum collecting plate for 5 hours to obtain a nonwoven base. The resultant nonwoven fabric substrate was washed with ethanol and then dried in a vacuum oven at room temperature for 24 hours to finally prepare a nonwoven fabric substrate having an average pore size of 11.6 占 퐉.

The nonwoven fabric substrate prepared above was immersed in 0.4 wt% of carboxymethylcellulose solution prepared by dissolving carboxymethylcellulose in a mixed solvent of ethanol and water at a weight ratio of 20:80 for 10 seconds, and then dried at 80 ° C for 1 hour, A composite nonwoven fabric having a pore size of 4.9 mu m and a thickness of 159 mu m was produced. At this time, the amount of carboxymethyl cellulose to be loaded was 21 parts by weight based on 100 parts by weight of the nonwoven fabric.

Example 2

An electrospinning solution was prepared by dissolving lactic acid-glycolic acid copolymer (PLGA) (lactic acid: glycolic acid = 70:30 by weight) in a mixed solvent of dimethylformamide (DMF) and chloroform (weight ratio = 1: 9) Prepared.

Thereafter, a voltage of 20 kV, a radiation distance of 20 cm, and a fluid velocity of 6 ml / h were fixed by using an electrospinning device, and the resultant was spun on a rotary drum collecting plate for 6 hours to obtain a nonwoven base. The resultant nonwoven fabric substrate was washed with ethanol and then dried in a vacuum oven at room temperature for 24 hours to obtain a nonwoven fabric substrate having an average pore size of 7 μm and calendered at a room temperature of 500 psi to obtain an average pore size of 4.1 μm Nonwoven substrate was finally prepared.

The nonwoven fabric substrate prepared above was immersed in 0.4 wt% of carboxymethylcellulose solution prepared by dissolving carboxymethylcellulose in a mixed solvent of ethanol and water at a weight ratio of 20:80 for 10 seconds, and then dried at 80 ° C for 1 hour, A composite nonwoven fabric having a pore size of 3.1 탆 and a thickness of 104 탆 was prepared. At this time, the amount of carboxymethyl cellulose to be loaded was 14 parts by weight based on 100 parts by weight of the nonwoven fabric.

Example 3

An electrospinning solution was prepared by dissolving lactic acid-glycolic acid copolymer (PLGA) (lactic acid: glycolic acid = 70:30 by weight) in a mixed solvent of dimethylformamide (DMF) and chloroform (weight ratio = 1: 9) Prepared.

Thereafter, a voltage of 20 kV, a radiation distance of 19 cm and a fluid velocity of 6 ml / h were fixed by using an electrospinning device, and the resultant was spin-coated on a rotary drum collecting plate for 8 hours to obtain a nonwoven base. The resultant nonwoven fabric substrate was washed with ethanol and then dried in a vacuum oven at room temperature for 24 hours to prepare a nonwoven fabric substrate having an average pore size of 5.4 μm.

The nonwoven fabric substrate prepared above was immersed in 0.4 wt% of carboxymethylcellulose solution prepared by dissolving carboxymethylcellulose in a mixed solvent of ethanol and water at a weight ratio of 20:80 for 10 seconds, and then dried at 80 ° C for 1 hour, A composite nonwoven fabric having a pore size of 1.9 mu m and a thickness of 181 mu m was produced. At this time, the amount of carboxymethyl cellulose to be loaded was 20 parts by weight based on 100 parts by weight of the nonwoven fabric.

Example 4

Polycaprolactone was dissolved in a mixed solvent of methylformamide (DMF) and chloroform (weight ratio = 3: 7) so as to be 12% by weight to prepare an electrospinning solution.

Thereafter, the nonwoven fabric substrate was obtained by fixing the filament at a voltage of 20 kV, a radiation distance of 20 cm, and a fluid velocity of 5 ml / h by using an electrospinning apparatus, and spinning it on a rotating drum collecting plate for 6 hours. The resultant nonwoven substrate was then subjected to a vacuum oven at 45 캜 for 24 hours to prepare a nonwoven substrate.

The nonwoven fabric substrate prepared above was immersed in 0.04% by weight of carboxymethylcellulose solution prepared by dissolving carboxymethylcellulose in a mixed solvent of ethanol and water at a weight ratio of 30:70 for 10 seconds and dried at 40 ° C for 30 minutes to obtain an average A composite nonwoven fabric having a pore size of 4.6 탆 and a thickness of 78 탆 was prepared.

Comparative Example 1

A nonwoven substrate prepared in the same manner as in Example 1 was prepared, except that the step of immersing the carboxymethylcellulose solution was not further carried out.

Comparative Example 2

A nonwoven substrate prepared in the same manner as in Example 3 was prepared, except that the step of immersing the carboxymethylcellulose solution was not further carried out.

Comparative Example 3

A composite nonwoven fabric substrate was prepared in the same manner as in Example 1, except that only water was used instead of ethanol and water miscible solvent in the preparation of the carboxymethylcellulose solution in the immersion treatment in the carboxymethylcellulose solution.

Character rating

Average pore size measurement

The pore size of the nonwoven fabric base material, the composite nonwoven fabric, and the nonwoven fabric base materials prepared in Comparative Examples 1 and 2 prepared in Examples 1 to 3 was measured using a capillary flow porometer (CFP-1200AEL, Porous Materials Inc.) The size was measured.

Hydrophilicity evaluation (contact angle)

The angle of contact is measured on the basis of the KS L 2110 standard using an image analyzer (DSA 100, KRUSS GmbH) using an angle analyzer (DSA 100, KRUSS GmbH) to measure the angle between the liquid surface and the solid surface formed by dropping 2-5 μl of deionized water on the non- Respectively. The hydrophilicity of the nonwoven fabric prepared in Example 1 and Comparative Example 1 was evaluated using the above evaluation method, and the results are shown in FIG.

Absorption magnification evaluation

Cut 3 cm ㅧ 3 cm of sample from the non-woven fabric under standard conditions and measure the weight accurately. The sample is immersed in 0.9% physiological saline for 30 seconds. Thereafter, one end of the nonwoven fabric is pulled out with a pair of tweezers, then waited until the physiological saline solution no longer falls off, and the weight is measured at the time of absorption, and the absorption magnification is calculated by the following formula.

Absorption magnification (g / g)

= [(Weight of sample after liquid absorption g) - (weight of sample before liquid absorption)] / (weight of sample before liquid absorption g)

Using the above-mentioned evaluation method, the absorption magnifications of the nonwoven fabric prepared in Examples and Comparative Examples were evaluated, and the results are shown in Table 1 below.

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Absorption magnification (g / g) 8.4 6.1 8.7 6.0 2.7 2.4

Evaluation of transparency during absorption

(1) Visual evaluation

The transparency of the composite nonwoven fabric prepared in Example 1 was visually evaluated after applying the 0.9% physiological saline solution to the wounds and the substrate for 30 seconds (left image), and then observing the transparency 2 and 3, respectively.

The nonwoven fabric prepared in Example 1 and Comparative Example 3 was visually evaluated for transparency after immersing 0.9% physiological saline solution for 30 seconds, and the photographs observed are shown in FIG.

2 to 4, in the case of the composite nonwoven fabric of Example 1, after the 0.9% physiological saline solution was absorbed for 30 seconds, the transparency was remarkably increased to such an extent that the object to be coated was completely shined, It can be seen that the transparency is completely different from that of Comparative Example 3 in which a carboxymethylcellulose solution is prepared using only water to form a carboxymethylcellulose coating layer.

(2) Evaluation of transparency by the reflectance measurement method

The composite nonwoven fabrics prepared in Examples 1 and 3 and the nonwoven fabric substrates prepared in Comparative Examples 1 and 2 were immersed in 0.9% physiological saline solution for 30 seconds and then exposed to a visible light wavelength range under a D65 standard light source using a Gretag Macbeth colorimeter (CE 3100) By using the reflectance measuring method at 400 to 700 nm.

O _p = 100 -? R _i / j

O _p : transparency (%)

Reflectance corresponding to R _i = i ( i = 1 to j ) th wavelength value

j = number of reflectance measurement times

The results are shown in Table 2 below.

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Transparency (%) 80.8 83.3 82.0 80.8 55.6 37.1

(3) Surface observation of composite nonwoven fabric

SEM photographs of the surface of the composite nonwoven fabric prepared in Example 1 and Comparative Example 3 are shown in FIGS. 5 and 6, respectively.

5 and 6, when the solvent used for the carboxymethyl cellulose solution for forming the carboxymethyl cellulose coating layer is a mixed solvent of water and ethanol, the carboxymethyl cellulose uniformly penetrates between the electrospun fibers, It can be seen that, in the case of a single solvent, carboxymethylcellulose is non-uniformly distributed in a very small part. This is because when a nonwoven fabric made of electrospun biodegradable polymer exhibits hydrophobicity and water having a large surface tension is used as a sole solvent, it is hydrophilic and penetration of aqueous solution of carboxymethylcellulose becomes difficult. On the other hand, when a mixed solvent of alcohol and water is used, surface tension is reduced and penetration into hydrophobic nonwoven fabrics becomes easy.

Claims (14)

2) polycaprolactone fiber and polylactic acid fiber, 3) polycaprolactone fiber and lactic acid-glycolic acid copolymer fiber, or 4) polycaprolactone fiber, polylactic acid fiber and polylactic acid fiber formed by electrospinning, And a lactic acid-glycolic acid copolymer fiber; And
A carboxymethyl cellulose coating layer formed on at least one of the both surfaces of the nonwoven fabric substrate or the inner pores of the nonwoven fabric substrate,
It is opaque in the non-liquid-absorbing state, becomes transparent in the liquid-absorbing state,
Wherein the composite nonwoven fabric has a transparency of 60% or more after being immersed in 0.9% physiological saline for 30 seconds. The method according to claim 1,
Wherein the composite nonwoven fabric has an average pore size of 5 m or less. The method according to claim 1,
Wherein the fibers have an average diameter of 100 to 4,000 nm. The method according to claim 1,
Wherein the content of lactic acid in the lactic acid-glycolic acid copolymer is 10 to 90 molar ratio. The method according to claim 1,
Wherein a loading amount of the carboxymethyl cellulose coating layer is 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric base material. delete The method according to claim 1,
Wherein the composite nonwoven fabric has a water absorption magnification of 4 g / g or more. 1) Polycaprolactone, 2) Polycaprolactone and polylactic acid, 3) Polycaprolactone and lactic acid-glycolic acid copolymer, or 4) Polycaprolactone, polylactic acid and lactic acid-glycolic acid copolymer are dissolved in a solvent Preparing an electrospinning solution;
Electrospinning the electrospinning solution to form a nonwoven substrate; And
And coating a carboxymethyl cellulose solution on the nonwoven fabric substrate to form a carboxymethylcellulose coating layer,
Wherein the composite nonwoven fabric has a transparency of 60% or more after being immersed in 0.9% physiological saline for 30 seconds. 9. The method of claim 8,
Wherein the carboxymethyl cellulose solution is prepared by dissolving carboxymethyl cellulose in water and a mixed solvent of a non-solvent and a non-solvent having a surface tension lower than that of water, wherein the carboxymethyl cellulose solution is free of carboxymethyl cellulose. 10. The method of claim 9,
Wherein the content of the non-solvent in the mixed solvent is 5 to 60% by weight. 10. The method of claim 9,
Wherein the non-woven fabric of carboxymethyl cellulose is at least one selected from the group consisting of alcohol, acetone, methylene chloride, and chloroform. 9. The method of claim 8,
Further comprising the step of calendering the nonwoven fabric substrate before or after coating the carboxymethylcellulose solution after forming the nonwoven fabric substrate by electrospinning. A sanitary article comprising the composite nonwoven fabric of any one of claims 1 to 5 and 7. The sanitary article according to claim 13, wherein the sanitary article is a medical covering material, an absorbent sanitary article, a food packaging material, or a mask pack.

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