KR101771934B1 - Maskpack including hydrophilic polymer nanofiber on both sides of a cellulose substrate and its manufacturing method - Google Patents

Abstract

The present invention relates to a mask pack in which a nanofiber layer formed by electrospinning a hydrophilic polymer solution on both sides of a cellulose substrate is laminated, and the bond between the substrate and the nanofiber layer is promoted to thereby suppress the elimination phenomenon as much as possible, And it has an advantage that the impregnation efficiency of the moisturizing component and various influential components is high and the manufacturing process can be simplified by rotating the upper and lower sides of the substrate by 180 ° in the manufacturing process.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a mask pack including a hydrophilic polymer nanofiber layer on both sides of a cellulosic substrate,

The present invention relates to a mask pack including a nanofiber and a method of manufacturing the same, and more particularly, to a mask pack including a nanofiber layer produced by electrospinning a hydrophilic polymer solution on both sides of a cellulose substrate.

Recently, environmental pollution caused by industrialization has caused a sudden increase in atopic skin patients and side effects such as skin damage due to exposure to ultraviolet rays due to ozone layer destruction.

Therefore, in order to remove wastes from damaged skin as described above, or to remove unnatural substances such as cucumber, citrus, aloe, carrot, wormwood, seaweed, carrot, ginseng, red ginseng, Potatoes, cacti, mesyl, vitamins, etc.) and minerals (elvan) have already been commercialized and marketed.

However, in the conventional mask pack, the nanofiber layer is merely laminated on the substrate and thermally fused, so that not only the substrate and the nanofiber layer can not be bonded together but also the retention time of the skin moisturizing component and the nutrient component is not constant.

The present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a mask pack including a nanofiber layer produced by electrospinning a hydrophilic polymer solution on both sides of a cellulose substrate.

In order to solve the above problems,

A cellulose substrate;

A first nano fiber layer formed by electrospinning a hydrophilic polymer solution selected from polyacrylonitrile, polyvinyl alcohol, polyamide, and hydrophilic polyurethane formed on one side of the cellulose substrate;

A second nanofiber layer formed by electrospinning the same polymer solution as the first nanofiber layer adhered to the other side of the polyethylene terephthalate substrate; Include

Wherein the polyethylene terephthalate base material and the nano fiber layer are bonded through an adhesive layer formed by electrospinning a low melting point polymer solution.

The low melting point polymer solution is selected from at least one selected from a low melting point polyester, a low melting point polyurethane, and a low melting point polyvinylidene fluoride,

The low melting point polymer solution is electrospun on the entire surface or a part of the substrate.

The mask pack manufactured according to the present invention can minimize the desorption phenomenon due to the presence of the cellulose base material and the nano fiber interlayer adhesive layer. The presence of the nano fiber layer significantly improves the skin adhesion, It has high efficiency and excellent spreading effect through the skin.

Further, the electrospinning apparatus for manufacturing the mask pack of the present invention includes a flip device for rotating the substrate 180 degrees above and below, thereby simplifying the process of electrospinning both surfaces of the substrate.

1 is a side view schematically showing an electrospinning apparatus according to the present invention,
2 is a side sectional view schematically showing a nozzle of a nozzle block installed in a unit of the electrospinning apparatus according to the present invention,
3 is a schematic view of a nozzle block installed in a spinning liquid unit of an electrospinning device according to the present invention,
4 is a perspective view schematically showing a state in which an electric heater is installed in a nozzle block installed in each unit of the electrospinning apparatus according to the present invention,
5 is a cross-sectional view taken along line A-A 'of FIG. 4;
6 is a perspective view schematically showing a nozzle block installed in a low melting point polymer unit of an electrospinning device according to the present invention,
FIG. 7 to FIG. 10 are plan views schematically illustrating an operation process of electrospinning a polymer spinning solution on the same plane of a substrate through nozzles of each nozzle tube of an electrospinning device for manufacturing a nanofiber web according to the present invention. FIG.
FIGS. 11 and 12 are plan views schematically illustrating an operation process of sequentially injecting a low melting point polymer and a polymer spinning solution through arrangement of a nozzle block in the low melting point polymer unit as shown in FIG. 6,
13 is a view showing a state in which the nozzle blocks provided in the low melting point polymer unit of the electrospinning apparatus according to the present invention are arranged in different shapes,
FIGS. 14 and 15 are diagrams illustrating an operation process of sequentially injecting a low-melting-point polymer and a polymer spinning solution according to the arrangement of the nozzles as shown in FIG. 13;
16 is a view showing a state in which the nozzle blocks provided in the low melting point polymer unit of the electrospinning apparatus according to the present invention are arranged in another form,
FIGS. 17 and 18 are diagrams showing an operation process in which the low melting point polymer and the polymer spinning solution are sequentially injected according to the arrangement of the same nozzle as shown in FIG. 16;
19 is a front view showing a laminated structure of a nanofiber filter manufactured by the present invention,
20 is a perspective view schematically showing a flip device of an electrospinning device according to the present invention,
21 to 24 are views schematically showing the operation of the flip device of the electrospinning device according to the present invention,
25 is a perspective view showing the wearing state of the mask pack of the present invention.

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

The present invention is not limited to the scope of the present invention, but is merely an example, and various modifications can be made without departing from the technical spirit of the present invention.

1 is a side view schematically showing an electrospinning apparatus according to the present invention. The electrospinning apparatus 1 according to the present invention comprises a bottom-up electrospinning apparatus 1, wherein at least one low-melting polymer unit 10a, 10c and a spinning liquid unit 10b, And the low melting point polymer units 10a and 10c and the spinning solution units 10b and 10d electrify the low melting point polymer or the polymer spinning solution individually.

The low melting point polymer units 10a and 10c electrospun a low melting point polymer solution for forming an adhesive layer and the spinning solution units 10b and 10d electrospun the polymer solution for forming a nanofiber layer.

The flip device 110 provided between the spinning liquid unit 10b and the low melting point polymer unit 10c of the electrospinning apparatus 1 is used to move the upper and lower surfaces of the base material Is rotated 180 degrees. That is, after passing through the spinning solution unit 10b, a fabric composed of a base material and the first polyvinylidene fluoride nanofiber nonwoven fabric laminated on the base material is supplied to the flip device 110, and in the flip device 110, The top surface of the fabric is shifted to the bottom surface and the top and bottom of the fabric are rotated 180 so that the bottom surface of the fabric is repositioned to the top surface.

The low melting point polymer solution electrospun in the low melting point polymer units (10a, 10c) is electrospun to form an adhesive layer to enhance adhesion between the substrate, the nano fiber layer, and the nano fiber layer, and to prevent desorption.

The low melting point polymer solution electrospun in the low melting point polymer units 10a and 10c is characterized by being a low melting point polyester, a low melting point polyurethane, and a low melting point polyvinylidene fluoride.

In the present invention, cellulose is used as a substrate.

As described above, the low melting point polymer solution electrospun in the low melting point polymer units 10a and 10c of the present invention is selected from a low melting point polyester, a low melting point polyurethane, and a low melting point polyvinylidene fluoride.

The low melting point polyurethane uses a low degree of polymerization polyurethane having a softening temperature of 80-100.

The low melting point polyester is preferably terephthalic acid, isophthalic acid or a mixture thereof. It is also possible to add ethylene glycol as a diol component to further lower the melting point.

The low melting point polyvinylidene fluoride uses a low melting point polyvinylidene fluoride having a weight average molecular weight of 5,000 and a melting point of 80 to 160.

It is needless to say that the low melting point polyurethane, the low melting point polyester and the low melting point polyvinylidene fluoride may be used singly or in combination of two or more.

The low-melting-point polymer unit and spinning solution unit may include a main tank 8 in which a low-melting-point polymer or polymer solution is filled, and a low-melting-point polymer or polymer solution for filling in the main tank 8 in a fixed amount (11) in which a plurality of nozzles (12) in the form of a pin are arranged and a low-melting-point polymer or polymer solution to be filled in the main tank (8) A collector 13 spaced at a predetermined distance from the nozzle 12 and a voltage generator 14a, 14b, 14c, 14d for generating a voltage in the collector 13 to accumulate the polymer spinning solution injected from the collector 12 .

With the above configuration, the low-melting-point polymer solution or spinning solution supplied from the main tank is electrospun to form an adhesive layer and a nanofiber layer.

2, the nozzle 12 provided in the nozzle block 11 of the electrospinning device 1 according to the present invention comprises a multi-tubular nozzle 500, and two or more kinds of polymer spinning solution Two or more inner and outer tubes 501 and 502 are combined in a sheath-core form so as to be able to radiate electrons simultaneously.

3 schematically shows a nozzle block installed in a spinning liquid unit of an electrospinning apparatus according to the present invention. As shown in the figure, a temperature regulating device 60 is installed in the tubular body 40 of the nozzle block 11, which is installed in each of the units, and in which a polymer solution is supplied to a plurality of nozzles 12 provided on the unit do.

Here, the flow of the polymer solution in the nozzle block 11 is supplied to each tube 40 from the main tank 8 in which the polymer solution is stored, through the solution flow pipe.

The polymer spinning solution supplied to each tube 40 is discharged and injected through a plurality of nozzles 12 and accumulated on the long sheet 15 in the form of nanofibers.

A plurality of nozzles 12 are mounted at predetermined intervals in the longitudinal direction on each of the tubes 40. The nozzles 12 and the tubes 40 are electrically connected to the tube 40 .

In order to control the temperature control of the polymer solution, the temperature control device 60 is formed of a heat ray 41 or a pipe provided at the periphery of the tube 40.

Fig. 4 is a perspective view schematically showing a state in which an electric heater is installed in a nozzle block installed in each unit of the electrospinning apparatus according to the present invention, and Fig. 5 is a sectional view taken along the line A-A 'in Fig. As shown in the figure, a thermostat device in the form of a heat line 41 is formed in a spiral shape on the periphery of the tubular body 40 of the nozzle block 11 so as to control the temperature of the polymeric spinning solution supplied to and introduced into the tubular body 40 .

Due to the above-described temperature control device, the temperature of the electrospinning can be performed at a high temperature (50 to 100) compared with a normal temperature. Conventional electrospinning is carried out at room temperature, but there is a problem in that the solute of the polymer solution is insoluble in the solvent at room temperature. Therefore, MEK (methyl ether ketone), THF (tetrahydrofuran), and alcohol diluent are used to easily prepare the polymer solution.

However, in the method using the diluent described above, the concentration of the solute is lowered to lower the efficiency of electrospinning, and problems such as environmental contamination due to the generation of an excessive residual solvent and an increase in the unit cost of production have been caused. In order to solve the problem of electrospinning at room temperature, a temperature regulating device 60 in the form of a heat ray 41 is formed in a spiral shape around the inner periphery of the tubular body 40 of the nozzle block 11, And the temperature of the polymer solution was controlled.

6 is a perspective view schematically showing a nozzle block installed in a low melting point polymer unit of an electrospinning apparatus according to the present invention. The nozzle arranged in the low melting point polymer unit may be applied to the front face portion of the substrate, but is preferably applied to a specific portion of the substrate if necessary. In Fig. 6, the nozzles are divided into five groups of nine nozzles, one at the center and two at the bottom in the upper part. However, the arrangement of the nozzle and the nozzle block is not limited thereto, and it is obvious that those skilled in the art can appropriately design, change and arrange the nozzle in consideration of the number of the nozzles and the amount of the low melting point polymer to be radiated.

FIGS. 7 to 10 are plan views schematically showing an operation process of electrospinning a polymer spinning solution on the same plane of a substrate through nozzles of each nozzle tube of an electrospinning device for manufacturing a nanofiber web according to the present invention. The nozzle tubes 112a, 112b, 112c, 112d, 112e, 112f, 112g, 112h, and 112i having a plurality of nozzles 111a linearly arranged on the upper surface thereof are connected to the substrate 115 on the nozzle block 111, 112b, 112c, 112d, 112e, 112f, 112g, 112h, 112i are connected to the spinning liquid main tank 8, The polymer spinning solution filled in the tank 8 is supplied.

The nozzle tubes 112a, 112b, 112c, 112d, 112e, 112f, 112g, 112h and 112i are connected to the spinning liquid main tank 8 through a supply pipe 240, A plurality of nozzle tubes 112a, 112b, 112c, 112d, 112e, 112f, 112g, 112h, 112i and a spinning liquid main tank 8 are branched.

At this time, the supply pipe 240, which is communicated to the nozzle tubes 112a, 112b, 112c, 112d, 112e, 112f, 112g, 112h, 112i in the spinning liquid main tank 8, , And the radiation amount regulating means comprises valves (212, 213, 214, 233).

The means for regulating the amount of radiation comprises valves 212, 213, 214 and 233.

By providing the valves 212, 213, 214 and 233 as the radiation amount adjusting means, it is possible to supply the respective nozzles 111a from the supply pipe 240 by opening and closing the valves 212, 213, 214 and 233 The valves 212, 213, 214 and 233 are controllably connected to a controller (not shown), and the valves 212, 213, 214, It is also possible that the opening and closing of the valves 212, 213, 214, and 233 are manually controlled according to the situation of the field and the operator.

The MD direction used in the present invention means a machine direction, and means a longitudinal direction corresponding to a traveling direction when continuous fabrics such as a film or a nonwoven fabric are produced. A CD direction is a cross direction, and a direction perpendicular to the MD direction do. MD is also referred to as machine direction / longitudinal direction, and CD is referred to as width direction / transverse direction.

Basis Weight or Grammage is defined as the mass per unit area, that is, the preferred unit, grams per square meter (g / m 2). In recent years, for the purpose of making the air filter and the unit lighter and more compact, a type of the filter having a smaller depth is required, and if the filter material having the same filtration area is put in the unit, the filter material faces contact each other due to the thickness of the filter material, There has been a problem in that the pressure loss of the air filter unit remarkably increases. To solve this problem, there has been an attempt to reduce the thickness of the filter material for the air filter, that is, to reduce the basis weight. However, such an attempt has been made to reduce the basis weight of the filter, and it is possible to solve the pressure loss of the air filter unit sufficiently when the basis weight is reduced for a specific portion of the filter for each specific industrial field to which the filter is applied. The strength of the filter medium can be maintained.

FIGS. 11 and 12 are plan views schematically showing an operation sequence in which the low melting point polymer and the polymer spinning solution are sequentially injected through the arrangement of the nozzle blocks in the low melting point polymer unit as shown in FIG. 6. In FIG. 5, The low melting point polymer is applied to a portion of the substrate (one at the center and two at the top and two at the top) and then the polymer spinning solution is radiated to the front side of the substrate.

13 and Fig. 16 show a state in which the nozzle blocks provided in the low melting point polymer unit of the electrospinning apparatus according to the present invention are arranged in another form. Fig. 13 is arranged to face the longitudinal direction MD of the substrate, and Fig. 16 shows the shape arranged to face the width direction CD of the substrate. The operation of sequentially spraying the low-melting-point polymer and the polymer solution according to the spray of the nozzle as shown in FIGS. 13 and 16 is shown in FIGS. 14 and 15 and FIGS. 17 and 18, respectively.

Hereinafter, a process in which the substrate is rotated 180 times according to the operation of the flip device 110 will be described in more detail.

20 to 24, a base material 15, through which the polymeric spinning solution is passed through the low-melting-point polymer units 10a, 10b and the polymer spinning solution is electrospun and the nano fiber layer is laminated, Having guide grooves 112 and 112 'for being inserted and guided at opposite ends of the base material 15, respectively, which are formed to be inwardly protruded inward from the inner periphery of both sides in the horizontal direction of the flip device 110 positioned at the rear end of the flip device 110, And is rotated 180 degrees while being transported along the right guide members 111 and 111 'so that the upper and lower surfaces thereof are reversed to the lower and upper positions.

At this time, the base material 15 is conveyed upward along the left guide member 111 out of the guide members 111 and 111 'protruding inward from the inner periphery of the flip device 110 at either end And the other end of the base material 15 is transported downward along the right guide member 111 'and then transported upward again, The substrate 15 inserted into the guide grooves 112 and 112 'of the left and right guide members 111 and 111' is positioned on the left and right guide members 111 and 111 ' And then rotated 180 degrees.

By the above-described structure, the polymer solution is passed through the units 10a, 10b located at the tip ends of the units 10a, 10b, 10c, 10d of the electrospinning apparatus 1, The substrate 15 on which the nanofiber layer is laminated and formed by electrospinning is rotated by 180 ° so that the polymer 15 is irradiated with the polymer solution when the units 10c and 10d located on the downstream side pass through the substrate 15, The spinning solution can be electrospun to form a laminate of nanofiber layers.

That is, by rotating the base material 15 by 180 with the flip device 110, the units 10a, 10b positioned at the tip ends of the units 10a, 10b, 10c, 10d of the electrospinning device 1, The polymeric spinning solution is electrospun on one side of the substrate 15 to form a laminate of the nanofiber layers and the unit 10c, 10d positioned on the rear end side of each unit 10a, 10b, 10c, The nano fiber layer can be laminated on both surfaces of the substrate 15 by electrospinning the polymer spinning solution on the other side of the substrate 15 to form a nano-island layer.

Example 1

Low-molecular-weight polymer solution was prepared by dissolving low-molecular-weight polyurethane in a solvent of DMAc (N, N-dimethylaceticamide) in an amount of 25% by weight, and put into the main tank of the low melting point polymer unit 10a or 10c of the electrospinning apparatus. Subsequently, polyacrylonitrile having a weight average molecular weight (Mw) of 157,000 and polyvinyl alcohol were dissolved in the same solvent of dimethylacetamide (N, N-dimethylacetamide, DMAc) to prepare a spinning liquid. 10d). In the low melting point polymer unit, an adhesive layer having a basis weight of 0.1 g / m ² was formed on the cellulose substrate by electrospinning the distance between the electrode and the collector at 40 cm, an applied voltage of 20 kV, and 70 ° C, The first nanofiber layer having a basis weight of 0.5 g / m ² was laminated by electrospinning at a distance of 40 cm and an applied voltage of 15 kV at 70 ° C. Thereafter, the substrate including the substrate and the first nanofiber layer laminated on the substrate was passed through a flip device, and the substrate was rotated so that the upper and lower sides were inverted by 180 °. Thereafter, the substrate was transferred to the low melting point polymer unit 10c, And a second nano fiber layer having a basis weight of 0.5 g / m ² was laminated by forming a distance between the electrode and the collector in the spinning solution unit 10 d by electrospinning at a distance of 40 cm, an applied voltage of 25 kV, and a temperature of 70 캜.

[Comparative Example 1] Production of a mask pack in which no adhesive layer was formed

A mask pack was prepared in the same manner as in Example 1 except that no adhesive layer was formed.

[Evaluation Example 1] Separation test of the nanofiber layer

With respect to the mask pack samples prepared in Example 1 and Comparative Example 1, occurrence of the nanofiber decolorized layer was visually observed, and the results are shown in Table 1.

Sample Degradation of Nano Fiber Layer 1 day 3 days 5 days 7 days 9th 11th 15th Example 1 NO NO NO NO NO NO NO Comparative Example 1 NO Degradation occurred after 3 days

In the mask pack of the present invention, no nanofiber delamination occurred even after 15 days, but in the mask pack without the adhesive layer, nanofiber delamination occurred after three days.

[Evaluation Example 2] Skin adhesion test

The mask pack samples prepared in Example 1 and Comparative Example 1 were applied to skin surfaces of five subjects for 30 minutes to evaluate the degree of skin adhesion (peel resistance). A typical mask pack sample without nanofibers was used as a control and evaluated. The results are shown in Table 2.

Sample Skin adhesion Example 1 Good Comparative Example 1 Good Control group Bad

From the results shown in Table 2, it can be seen that the mask pack including the nanofiber layer exhibits better skin adhesion than the conventional non-woven mask pack as in the present invention.

[Evaluation Example 3] Skin soothing and moisturizing test

A mask pack was prepared in the same manner as in Example 1 except that hydrophilic polyvinylidene fluoride, polyvinyl alcohol (PAN), hydrophilic polyurethane (PU) and polyvinyl alcohol (PVA) were used as a polymer spinning solution.

The mask pack thus prepared was impregnated with the skin active component as shown in Table 3 below in weight percent.

Raw material name Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 PVDF Hydrophilic
PVDF PAN Hydrophilic
PU PVA Baby 1.8 1.8 1.8 1.8 1.8 Tataric acid 0.12 0.12 0.12 0.12 0.12 Butylene glycol 8 8 8 8 8 Carp glue sword 2.2 2.2 2.2 2.2 2.2 antiseptic 0.35 0.35 0.35 0.35 0.35 Spices 0.1 0.1 0.1 0.1 0.1 Chamomile extract 0.5 0.5 0.5 0.5 0.5 Ivy extract 0.5 0.5 0.5 0.5 0.5 Purified water Balance Balance Balance Balance Balance

After using the above Example 1 and Comparative Examples 2 to 5 for 10 patients three times, the degree of skin relaxation and moisturizing sensation was evaluated on a scale of 5 points: 5 points: very good, 4 points: slightly better, and 3 points : Average, 2: Poor, 1: Very poor, and the average value of each is shown in Table 4 as a result of skin soothing and moisturizing effect when using the product.

The degree of skin soothing and moisturizing effect with mask pack Example 1 4.5 Comparative Example 2 3.3 Comparative Example 3 3.2 Comparative Example 4 2.5 Comparative Example 5 2.7

As can be seen from the evaluation example, the mask pack manufactured according to the present invention is easier to adhere between the base layer and the polymer electrospinning layer than the conventional mask pack, and does not cause separation, and the skin adhesion And it has an advantage that the impregnation efficiency of the moisturizing component and various influential components is high and the diffusion effect through the skin is excellent.

1: electrospinning device, 3: feed roller,
5: take-up roller, 7: main control device,
8: spinning liquid main tank, 10a, 10b: unit,
11: nozzle block, 12: nozzle,
13: collector, 14, 14a, 14b: voltage generator,
15, 15a, 15b: long sheet, 16: auxiliary conveying device,
16a: auxiliary belt, 16b: auxiliary belt roller,
18: case, 19: insulating member,
30: Long sheet conveying speed adjusting device, 31: Buffer section,
33, 33 ': support roller, 35: regulating roller,
40: tube, 60: thermostat,
70: thickness measuring device, 80: air permeability measuring device,
90: laminating device, 110: flip device,
111, 111 ': guide piece, 112, 112': guide groove,
200: overflow device, 211, 231: stirring device,
212, 213, 214, 233: valve, 216: second transfer pipe,
218: second conveyance control device, 220: intermediate tank,
222: second sensor, 230: regeneration tank,
232: first sensor, 240: supply pipe,
242: supply control valve, 250: circulating fluid recovery path,
251: first transfer pipe, 300: VOC recycling apparatus,
310: condenser, 311, 321, 331, 332: piping,
320: distillation device, 330: solvent storage device.

Claims (6)

A cellulose substrate;
A first nano fiber layer formed by electrospinning a hydrophilic polymer solution selected from polyacrylonitrile, polyvinyl alcohol, polyamide, and hydrophilic polyurethane formed on one side of the cellulose substrate;
A second nanofiber layer formed by electrospinning the same polymer solution as the first nanofiber layer adhered to the other side of the cellulose substrate; Including,
The substrate and the nanofiber layer are bonded to each other through an adhesive layer formed by electrospinning a low melting point polymer solution,
Wherein the low melting point polymer solution is one selected from the group consisting of a low melting point polyester, a low melting point polyurethane, and a low melting point polyvinylidene fluoride. delete The method according to claim 1,
Characterized in that the low-melting-point polymer solution is electrospun on the entire surface or a part of the substrate The method according to claim 1,
Characterized in that the electrospinning of the hydrophilic polymer solution emits different weights in the MD direction or the CD direction. delete delete

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