KR102294965B1 - Hydrophilic modifying coating agent for non-woven having non-toxic to cells, Non-woven having non-toxic to cells and Manufacturing method thereof - Google Patents

Abstract

The present invention relates to a hydrophilic modified coating agent without cytotoxicity and a fiber product modified to be hydrophilic using the same, and more specifically, to a product having a hydrophobic surface, for example, a hydrophilic modified coating agent suitable for modifying a hydrophobic nonwoven fabric into hydrophilicity; It relates to a cell non-toxic nonwoven fabric manufactured using the same.

Description

Cell non-toxic hydrophilic modified coating agent for non-woven fabric, cell non-toxic non-woven fabric containing the same, and manufacturing method thereof

The present invention relates to a product having a hydrophobic surface with little cytotoxicity, for example, a hydrophilic modified coating agent suitable for modifying a hydrophobic nonwoven fabric into hydrophilicity, and a cytotoxic nonwoven fabric manufactured using the same.

Since the conventionally known nonwoven fabrics made of polyolefin materials such as polypropylene are strongly hydrophobic, there is a problem that their applications as industrial nonwovens and sanitary products requiring hydrophilicity are very limited.

In particular, nonwoven fabrics are used in hygiene products, such as disposable absorbent products such as baby diapers, adult diapers, sanitary napkins for women, and panty liners. As the non-woven fabric, most synthetic non-woven fabrics are applied, and as the synthetic non-woven fabrics, non-woven fabrics made of polyolefin materials such as polyethylene and polypropylene are applied. However, these hygiene products require hydrophilicity, and since the nonwoven fabric made of polyolefin material is hydrophobic, it is applied after imparting hydrophilicity to the nonwoven fabric.

In order to solve this problem, a synthetic hydrophilic modified coating agent is applied to the nonwoven fabric, but when used on the surface in contact with the skin, there is a problem in that the synthetic hydrophilic modified coating agent is not discharged and remains on the body. Moreover, the synthetic hydrophilic modified coating agent introduced through the skin cell membrane travels around the body through the blood, and there is a risk of causing disorders in cells such as the brain, heart, liver, and spleen, and there is a problem that may also cause atopic dermatitis.

Therefore, there is a need to develop a hydrophilic modified coating agent that is not harmful to the human body while imparting hydrophilicity to a product made of a hydrophobic material in direct contact with the human body, preferably a hydrophobic nonwoven fabric.

Republic of Korea Publication No. 10-2008-0041117 (published on April 23, 2018) Republic of Korea Registration Notice No. 1984-0001026 (published on July 20, 1984)

An object of the present invention is to solve the problems of these nonwovens based on the background of the problems of the conventional nonwovens as described above, and in detail, having an optimal composition and composition ratio with low cytotoxicity To prepare a hydrophilic modified coating agent, and to provide a non-toxic cell non-woven fabric that imparts hydrophilicity to the hydrophobic non-woven fabric using the same.

In order to solve the above problems, the cell-free hydrophilic modified coating agent of the present invention includes sodium salt, maleate, phosphate and an alcohol ether-based compound.

As a preferred embodiment of the present invention, the cell-free hydrophilic modification coating agent may include 15 to 20% by weight of sodium salt, 10 to 16% by weight of maleate, 2 to 8% by weight of phosphate, and the remainder of the alcohol ether-based compound. .

In a preferred embodiment of the present invention, the sodium salt in the composition of the cell-free hydrophilic modification coating agent is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy) ) poly(oxy-1,2-ethanediyl), sulfobutanedioxane 1,4-bis(2-(C ₁ to C ₃ alkyl) (C ₄ to C ₈ alkyl) ester sodium salt, sodium taloate, It may include at least one selected from sodium cocoate and sodium palm kernelate.

In a preferred embodiment of the present invention, in the composition of the non-toxic hydrophilic modifying coating agent, the maleate is bis(2-(C ₁ to C ₃ alkyl) (C ₄ to C ₈ alkyl) maleate, ethylene maleic anhydride It may include at least one selected from an acid copolymer and an isobutylene maleic anhydride copolymer.

In a preferred embodiment of the present invention, the phosphate in the composition of the non-toxic hydrophilic modifying coating agent is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphoric acid It may include at least one selected from tris(2-ethylhexyl)ester and (Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate.

As a preferred embodiment of the present invention, the alcohol ether compound in the composition of the non-toxic hydrophilic modification coating agent includes at least one selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol, and alcohol polyoxyethylene ether. can do.

As a preferred embodiment of the present invention, the non-toxic hydrophilic modified coating agent may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20° C.).

As a preferred embodiment of the present invention, a solution obtained by dissolving the non-toxic hydrophilic modified coating agent in water at a concentration of 10% by weight may have a pH of 5 to 8 (at 20° C. analysis).

As a preferred embodiment of the present invention, the non-toxic hydrophilic modified coating agent may have a melting point of -2 to 2 ℃.

Another object of the present invention relates to a method for manufacturing a non-toxic non-woven fabric using the cell-free hydrophilic modified coating agent described above, the first step of preparing the non-woven fabric; A second step of coating a part or the whole of the non-woven fabric with a non-toxic hydrophilic modified coating agent; and a third step of thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment to modify the nonwoven fabric to be hydrophilic.

In a preferred embodiment of the present invention, the nonwoven fabric may include hydrophobic fibers.

As a preferred embodiment of the present invention, the hydrophobic fiber may be a polyolefin-based fiber including at least one selected from among polyethylene fibers, polypropylene fibers, and propylene-ethylene copolymer fibers.

As a preferred embodiment of the present invention, the hydrophobic fiber may have an average diameter of 1 to 50 μm.

Another object of the present invention relates to a cell non-toxic non-woven fabric, wherein a part or all of the non-woven fabric containing hydrophobic fibers is modified with a hydrophilic non-woven fabric, wherein the cell non-toxic hydrophilic-modified coating agent is used in an amount of 0.1 to 3 wt % of the total weight of the non-woven fabric. may include

As a preferred embodiment of the present invention, _{when measuring IC 50} based on the ISO 10993-5 method, the cell viability may be 70 to 100%.

In a preferred embodiment of the present invention, the nonwoven fabric may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, a wet-laid, or a dry-laid nonwoven fabric.

The hydrophilic modified coating agent of the present invention has no cytotoxicity and has excellent coating properties, and when hydrophilic modification of a textile material product is used, it has low rewetting properties. Suitable for use in modifying hydrophobic fiber products into hydrophilic fibers. , particularly suitable for application to products that come into direct contact with the skin.

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

The non-toxic hydrophilic modified coating agent of the present invention includes sodium salt, maleate salt, phosphate salt and an alcohol ether-based compound.

The sodium salt is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethanediyl), sulfobutanedioxane sulfobutane Dioxane 1,4-bis(2-(C ₁ ~ C ₃ Alkyl) (C ₄ ~ C ₈ Alkyl) ester sodium salt, sodium taloate, sodium cocoate and sodium palm kernelate 1 or 2 types selected from may include the above, preferably octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethanediyl) and sulfobutanedioxane and sulfobutanedioxane 1,4-bis(2-(C ₁ to C ₃ alkyl) (C ₄ to C ₈ alkyl) ester sodium salt selected from one or two or more selected from the group consisting of , more preferably ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethanediyl) and sulfobutanedioxane sulfobutanedioxane 1,4-bis(2-(C ₂ to C ₃ of Alkyl) hexyl) may include one or two or more selected from the ester sodium salt.

And, the content of the sodium salt may include 15 to 20% by weight of the total weight of the hydrophilic modified coating agent, preferably 16 to 18.5% by weight, more preferably 16.5 to 18.0% by weight. At this time, if the sodium salt content is less than 15% by weight, there may be a problem that the pH of the modified coating agent is too low, and if it exceeds 20% by weight, the pH of the modified coating agent is rather high too high, and after reforming the nonwoven fabric, re-wetting is lowered There may be problems, so it is recommended to use it within the above range.

In the composition of the hydrophilic modifying coating agent, the maleate is bis(2-(C ₁ to C ₃ alkyl)(C ₄ to C ₈ alkyl) maleate, ethylene maleic anhydride copolymer and isobutylene maleic anhydride copolymer. may include one or two or more selected from, preferably selected from bis(2-(C ₂ to C ₃ alkyl) (C ₅ to C ₇ alkyl) maleate and ethylene maleic anhydride copolymer One or two types may be used, more preferably bis(2-(C ₂ to C ₃ alkyl)hexyl)maleate.

And, the content of maleic acid salt may include 10 to 16% by weight, preferably 11.0 to 14.8% by weight, more preferably 12.0 to 14.0% by weight based on the total weight of the hydrophilic modified coating agent. At this time, if the maleate content is less than 10% by weight, there may be a problem that the hydrophilicity improvement effect of the modified nonwoven fabric is lowered, and if it exceeds 16% by weight, there may be a problem of increased cytotoxicity. good.

Next, in the composition of the hydrophilic modification coating agent, the phosphate is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, tris(2-ethylhexyl) ester, ( Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate and poly(oxy-1,2-ethanedinyl), α-dodecyl-ω-hydroxy- , phosphate, potassium salt {Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6} may include one or two or more selected from among them.

And, the content of the phosphate may include 2 to 8% by weight, preferably 2.5 to 7.5% by weight, more preferably 3.0 to 6.2% by weight of the total weight of the hydrophilic modified coating agent. At this time, if the phosphate content is less than 2% by weight, there may be a problem in that the effect of improving the durable absorbency of the modified nonwoven fabric is insufficient, and if it exceeds 8% by weight, there may be a problem that the durable absorbency is lowered, so use within the above range good to do

Next, the alcohol ether compound in the composition of the hydrophilic modified coating agent serves as a solvent for other compositions of the hydrophilic modified coating agent, and is selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol and alcohol polyoxyethylene ether. It may include one or two or more, preferably one or two selected from dipropylene glycol monomethyl ether, polyvinyl ether, and alcohol polyoxyethylene ether, more preferably dipropylene glycol monomethyl ether and one or two selected from among alcohol polyoxyethylene ethers may be used.

And, the content of the alcohol ether-based compound is used in the remaining amount excluding other compositions of the total 100% by weight of the hydrophilic modified coating agent.

The cell non-toxic hydrophilic modified coating agent of the present invention prepared by mixing the above-described compositions may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20° C.), preferably 980 to 1,080 mPa. s, more preferably 1,000 to 1,060 mPa.s.

In addition, when the non-toxic hydrophilic modified coating agent of the present invention is dissolved in water at a concentration of 9 to 12% by weight, preferably at a concentration of 10% by weight, when analyzed at 20° C., the pH is 5 to 8, preferably pH 5.5 to 7.5, more preferably pH 5.8 to 7.0.

And, the cell non-toxic hydrophilic modified coating agent of the present invention may have a melting point of -3 to 3°C, preferably a melting point of -2 to 2°C.

A hydrophobic product can be modified to be hydrophilic by using the non-toxic hydrophilic modification coating agent described above, and as a preferred example, the hydrophilic modification of the nonwoven fabric is described as follows.

Step 1 of preparing a nonwoven fabric; A second step of coating a part or the whole of the non-woven fabric with a non-toxic hydrophilic modified coating agent; and a third step of thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment to modify the nonwoven fabric to be hydrophilic.

The nonwoven fabric of step 1 includes hydrophobic fibers, may include some hydrophilic fibers, or may be all nonwoven fabrics made of hydrophobic fibers. Some or all of the nonwoven may be hydrophobic.

The hydrophobic fiber may be a polyolefin-based fiber including at least one selected from among polyethylene fibers, polypropylene fibers, and propylene-ethylene copolymer fibers.

And, the hydrophobic fiber may have an average diameter of 1 μm to 50 μm, preferably 1 μm to 30 μm.

In addition, the nonwoven fabric of step 1 may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, a wet-laid, or a dry-laid nonwoven fabric.

Next, the cell non-toxic hydrophilic modified coating agent of the second step is the same as described above. In addition, the two-step coating may be performed by a general coating method used in the art, and preferably may be performed through a kiss roll coating method or a spray coating method.

Next, the three-step heat treatment may be performed by applying heat of 100 to 150 °C, preferably 110 to 140 °C, in a drum dryer. At this time, if the heat treatment temperature is less than 100 ℃ there may be a problem that the nonwoven fabric is less dried, if the heat treatment temperature exceeds 150 ℃, there may be a problem that the nonwoven fabric becomes hard.

The prepared non-toxic cell-modified hydrophilic non-woven fabric may include 0.1 to 3.0 wt% of the non-toxic hydrophilic modified coating agent, preferably 0.4 to 2.8 wt%, and more preferably 0.5 to 1.5 wt%. At this time, if the content of the non-toxic hydrophilic modifying coating agent is less than 0.1% by weight, the hydrophilic modification effect may be insignificant, and if it exceeds 3% by weight, the rewetting property of the nonwoven fabric increases and there may be a problem of moistening.

And, the cell non-toxic nonwoven fabric of step 3 may have a basis weight of 10 to 100 gsm.

In addition, the non-toxic cellulosic nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when measuring _{IC 50 based on the ISO 10993-5 method.}

In addition, according to WSP 70.3(08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine), the cell non-toxic nonwoven fabric of the present invention is 2.50 to 3.50 seconds, preferably 2.50 to 3.20 seconds, when the liquid absorption rate is measured. can

In addition, the cell non-toxic nonwoven fabric of the present invention has a durable absorbency of 1.50 to 2.80 seconds for the first time, and a second time when the durable absorbency is measured according to WSP 70.7(09) (Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time). Durable absorption may be 2.00 ~ 3.50 seconds, and the third durable absorption may be 2.30 ~ 3.80 seconds.

In addition, the cell non-toxic nonwoven fabric of the present invention has a rewetting property of 2.0 to 3.5 g, preferably 2.2 to when measuring rewetting to a liquid according to WSP 70.8 (09) (Standard Test Method for Wetback After Repeated Strike-Through Time). It may be 3.3 g.

In addition, the non-toxic cellulosic nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when measuring _{IC 50 based on the ISO 10993-5 method.}

Hereinafter, the present invention will be described in more detail based on examples. The following examples are provided to help the understanding of the present invention, and should not be construed as limiting the scope of the present invention by the examples.

[Example]

Example 1: Preparation of non-toxic hydrophilic modified coating agent

Sodium salt of sulfobutanedioxane 1,4-bis (2-ethylhexyl) ester sodium salt (cas no. 577-11-7), maleate of bis (2-ethylhexyl) maleate (bis (2-ethylhexyl) maleate, cas no. 142-16-5), phosphate poly (oxy-1,2-ethanedinyl), α-dodecyl-ω-hydroxy-, phosphate, potassium salt (Poly (oxy-1,2-) ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6) and dipropylene glycol monomethyl ether, an alcohol ether-based compound, are mixed and stirred to prepare a non-toxic hydrophilic modified coating agent did.

In addition, the contents of each of sodium salt, maleate, phosphate, and alcohol ether-based compounds in the hydrophilic modified coating agent are shown in Table 1 below.

Examples 2 to 7 and Comparative Examples 1 to 6

A hydrophilic modified coating agent was prepared in the same manner as in Example 1, but a hydrophilic modified coating agent having the composition and composition ratio as shown in Table 1 below was prepared, respectively.

division
(weight%) sodium salt maleate phosphate alcohol ether compounds Example 1 17.2 13.0 4.6 remaining balance Example 2 15.3 13.2 4.9 remaining balance Example 3 18.5 13.0 4.2 remaining balance Example 4 17.2 11.0 4.8 remaining balance Example 5 17.2 14.8 4.8 remaining balance Example 6 17.2 13.0 2.5 remaining balance Example 7 17.2 13.0 7.5 remaining balance Comparative Example 1 13.5 13.0 4.6 remaining balance Comparative Example 2 21.0 13.0 4.6 remaining balance Comparative Example 3 17.2 9.3 4.8 remaining balance Comparative Example 4 17.2 16.6 4.8 remaining balance Comparative Example 5 17.2 13.0 1.0 remaining balance Comparative Example 6 17.2 13.0 9.0 remaining balance

Comparative Example 7

Isopropyl alcohol was prepared as a hydrophilic modifying coating agent.

Comparative Example 8

A solution containing 20% by weight of the diester and the remaining amount of the propylene glycol compound was prepared as a hydrophilic modification coating agent.

Comparative Example 9

A siloxane-based hydrophilic modification coating agent (Dimethylsiloxane, 3-(3-((3-cocoamidopropyl)dimethylammonio)-2-hydroxyprpoxy)propyl groupterminated acetate / CAS 134737-05-6) was prepared as a hydrophilic modification coating agent;

Experimental Example 1: Measurement of viscosity and pH of hydrophilic modified coating agent

Viscosity and pH of each of the hydrophilic modified coating agents prepared in Examples 1 to 7 and Comparative Examples 1 to 9 were measured, and the results are shown in Table 2 below.

At this time, the viscosity was measured according to the ASTM D7042 standard test (20° C.), and the pH is the pH of a solution in which a hydrophilic modified coating agent is dissolved in water at a concentration of 10 wt %, and analyzed at 20° C.

division Viscosity
(mPa.s) pH Melting point (℃) Example 1 1,015 to 1,025 6.0 ~ 6.1 -1 to 1 Example 2 990 to 995 5.2 to 5.3 -1 to 1 Example 3 1,005 to 1,010 6.4 to 6.5 -1 to 1 Example 4 1,050 to 1,060 5.8 to 5.9 -1 to 1 Example 5 1,035 to 1,040 6.0 ~ 6.1 -1 to 1 Example 6 990 to 995 5.7 ~ 5.8 0 to 2 Example 7 1,080 to 1,085 6.2 to 6.3 -3 to -1 Comparative Example 1 980 to 985 4.5 to 4.6 -1 to 1 Comparative Example 2 1,070 ~ 1,075 7.4 to 7.5 -1 to 1 Comparative Example 3 985 ~ 990 6.5 to 6.7 -1 to 1 Comparative Example 4 1,095 to 1,100 5.7 ~ 5.8 -1 to 1 Comparative Example 5 975 to 980 5.7 ~ 5.8 3 to 5 Comparative Example 6 1,095 to 1,100 6.3 to 6.4 -3 to -1

Looking at the physical property measurement results of the modified coating agent in Table 2, Examples 1 to 7 showed an appropriate range of physical properties in the range of viscosity 990 to 1,060 mPa.s, pH 5.2 to 6.3, and melting point -3°C to 1°C.

On the other hand, in the case of Comparative Example 1 using less than 15% by weight of the sodium salt, compared with Examples 1 and 2, there was a problem that the pH was rapidly lowered and acidified, and the sodium salt was used in excess of 20% by weight. In the case of Example 2, compared with Examples 1 and 3, the pH showed a tendency to increase rapidly.

In addition, looking at the melting points of Examples 6 to 7 and Comparative Examples 5 to 6, it can be seen that the phosphate content affects the melting point of the modified coating agent. and Comparative Example 5 had the highest melting point, and comparing Example 7 and Comparative Example 6, there was a tendency that the melting point did not decrease even if the amount of phosphate exceeded 8 wt%.

Preparation Example 1: Preparation of hydrophilic modified non-toxic cellulosic nonwoven fabric

A spunbond nonwoven fabric having a basis weight of 18 gsm made of polypropylene fibers having an average diameter of 17 μm was prepared (manufacturer Toray Advanced Materials, trade name LIVSEN).

Next, the hydrophilic modified coating agent prepared in Example 1 was coated with a nonwoven fabric by a kiss roll coating method and dried.

Next, a non-toxic cellulosic nonwoven fabric modified to be hydrophilic was prepared by heat treatment under a temperature condition of about 125 to 130° C. in a drum dryer.

The content of the hydrophilic-modified coating agent in the prepared cell non-toxic nonwoven fabric was about 0.7% by weight.

Preparation Examples 2 to 7 and Comparative Preparation 1 to 11

A hydrophilic modified nonwoven fabric was prepared in the same manner as in Preparation Example 1, but instead of the hydrophilic modified coating agent of Example 1, each of the nonwoven fabrics modified to be hydrophilic using each of the hydrophilic modified coating agents prepared in Examples 2 to 5 and Comparative Examples 1 to 9 was prepared, and Preparation Examples 2 to 7 and Comparative Preparation Examples 1 to 11 were carried out, respectively, as shown in Table 3 below.

division Types of hydrophilic modified coatings Content in non-woven fabric Preparation Example 1 Example 1 0.7 wt% Preparation 2 Example 1 0.4% by weight Preparation 3 Example 1 2.6 wt% Preparation 4 Example 2 0.7 wt% Preparation 5 Example 3 0.7 wt% Preparation 6 Example 4 0.7 wt% Preparation 7 Example 5 0.7 wt% Preparation 8 Example 6 0.7 wt% Preparation 9 Example 7 0.7 wt% Comparative Preparation Example 1 Example 1 0.08 wt% Comparative Preparation Example 2 Example 1 3.1 wt% Comparative Preparation Example 3 Comparative Example 1 0.7 wt% Comparative Preparation Example 4 Comparative Example 2 0.7 wt% Comparative Preparation Example 5 Comparative Example 3 0.7 wt% Comparative Preparation Example 6 Comparative Example 4 0.7 wt% Comparative Preparation Example 7 Comparative Example 5 0.7 wt% Comparative Preparation Example 8 Comparative Example 6 0.7 wt% Comparative Preparation Example 9 Comparative Example 7 0.7 wt% Comparative Preparation Example 10 Comparative Example 8 0.7 wt% Comparative Preparation Example 11 Comparative Example 9 0.7 wt%

Experimental Example 1: Evaluation of liquid absorption rate (Strike through)

A measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Examples and Comparative Preparation Examples to a size of 10 cm x 10 cm (width x length).

Thereafter, the absorption rate of the measurement sample (specifically, the liquid absorption rate of the hydrophilic nonwoven layer) was measured according to WSP 70.3(08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine), and the result was It is shown in Table 4 below. After measuring the absorbance 10 times for the same type of measurement sample, the average value was recorded as the final absorption rate. Specifically, after placing the measurement sample on the absorbent paper, the absorption rate was evaluated for the time to absorb all 5 ml of 0.9 wt% NaCl aqueous solution through the absorbent paper.

Experimental Example 2: Evaluation of Durable Absorption

A measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Examples and Comparative Preparation Examples to a size of 10 cm x 10 cm (width x length).

Thereafter, the durable absorbance (specifically, the repeat absorbency of the hydrophilic nonwoven layer) of the measurement sample was measured according to WSP 70.7(09) (Standard Test Method for Nonwoven- Repeated Liquid Strike-Through Time), and the results are shown below. Table 4 shows. After measuring the durable absorbance three times for the same type of measurement sample, the durable absorbance was recorded. Specifically, after placing the measurement sample on the absorbent paper, 5 ml of 0.9 wt% NaCl aqueous solution through the absorbent paper was evaluated for durable absorption for a total of 15 ml once, twice, and three times, and the evaluation record is 1, 2, and 3 times were recorded, respectively.

Experimental Example 3: Evaluation of re-wettability (RiŸ‡, Re-wet)

According to WSP 70.8(09) (Standard Test Method for Wetback After Repeated Strike-Through Time) using the measurement sample for which the absorption of the liquid was evaluated according to Experimental Example 1, the rewetting property of the measurement sample (specifically, hydrophilic nonwoven fabric) layer) was measured, and the results are shown in Table 4 below. Specifically, after placing a measurement sample for evaluating liquid absorption according to Evaluation Example 1 on a new absorbent paper, 20 ml of 0.9 wt% NaCl aqueous solution is placed on the absorbent paper, and after applying a load of 5 kg to the measurement sample, the measurement The amount of liquid reabsorbed back into the sample was measured and recorded as rewetting.

Experimental Example 4: Evaluation of cytotoxicity

_{Samples were collected from nonwoven fabrics prepared in Preparation Examples and Comparative Preparation Examples, and IC 50} (inhibition concentration 50, colony formation inhibition) according to ISO 10993-5 (Biological evaluation of medical devices-Part 5: Tests for in-vitro cytotoxicity). concentration) were analyzed, and the results are shown in Table 4 below. The IC ₅₀ evaluation result must be 70 to 100% to be evaluated as a non-toxic non-woven fabric.

division Non-woven
basis weight
(gsm) absorption
speed
(sec) endurance
Absorption (sec) rewetting
(g) IC ₅₀
(%) note 1 time Episode 2 3rd time Preparation Example 1 18 2.94 1.86 2.52 2.86 2.9 100 Cell non-toxic Preparation Example 2 18 3.15 2.50 3.27 3.41 2.2 100 Cell non-toxic Preparation 3 18 2.52 1.55 2.25 2.43 3.3 97 Cell non-toxic Preparation 4 18 2.87 1.79 2.40 2.72 2.9 100 Cell non-toxic Production Example 5 18 2.98 1.95 2.67 3.02 2.3 99 Cell non-toxic Preparation 6 18 3.18 2.35 3.07 3.28 2.7 100 Cell non-toxic Preparation 7 18 2.68 1.72 2.30 2.57 3.1 95 Cell non-toxic Preparation 8 18 3.04 2.08 2.88 3.12 2.7 100 Cell non-toxic Preparation 9 18 2.98 2.02 2.63 3.20 3.0 100 Cell non-toxic Comparative Preparation Example 1 18 4.42 3.28 4.92 5.59 1.2 100 Cell non-toxic Comparative Preparation Example 2 18 2.48 1.50 2.17 2.39 4.6 78 Moderate cytotoxicity Comparative Preparation Example 3 18 2.85 1.72 2.46 2.78 2.8 100 Cell non-toxic Comparative Preparation Example 4 18 3.05 2.09 2.98 3.10 1.7 100 Cell non-toxic Comparative Preparation Example 5 18 3.86 2.77 3.46 3.828 2.7 100 Cell non-toxic Comparative Preparation Example 6 18 2.36 1.52 1.98 2.21 3.2 81 Moderate cytotoxicity Comparative Preparation Example 7 18 3.09 2.14 2.95 3.27 2.6 100 Cell non-toxic Comparative Preparation Example 8 18 2.82 1.83 3.20 4.13 3.1 100 Cell non-toxic Comparative Preparation Example 9 18 3.02 2.10 2.72 4.40 3.8 39.7 medium
cytotoxicity Comparative Preparation Example 10 18 2.54 1.61 2.45 2.43 4.5 16.4 medium
cytotoxicity Comparative Preparation Example 11 18 2.91 2.90 2.64 3.16 4.2 68.5 Moderate cytotoxicity

Looking at the physical property measurement results in Table 4, in the case of Preparation Examples 1 to 9, the nonwoven fabric made of the hydrophobic fiber was modified to be hydrophilic, so that the fast liquid absorption rate, durability against repeated absorption (durable absorption) and rewetting were excellent. It can be confirmed that there is no cytotoxicity.

In contrast, in the case of Comparative Preparation Example 1 using less than 0.1% by weight of the hydrophilic modified coating agent, when compared to Preparation Examples 1 and 2, there is little hydrophilic modification effect, so the absorption rate, durability absorption and refolding properties are very poor showed results. In addition, in the case of Comparative Preparation Example 2 in which the hydrophilic modification coating agent was used in excess of 3.0% by weight, compared with Preparation Examples 1 and 3, the effect of increasing the hydrophilicity was weak, and the rewetting property was too high, so that the nonwoven fabric was rather damp, rather Only cytotoxicity increased.

In the case of Preparation Example 3 using the modified coating agent of Example 2 and Preparation Example 4 using the modified coating agent of Example 4, when compared with Preparation Example 1, there was no significant difference in terms of hydrophilic modification. On the other hand, in the case of Comparative Preparation Example 4 using the modified coating agent of Comparative Example 2, there was a problem in that the re-wetting property was significantly reduced as compared to Preparation Example 5.

In addition, in the case of Comparative Preparation Example 5 using the modified coating agent of Comparative Example 3, compared with Preparation Example 6 (using Example 4), the hydrophilicity improvement effect was lowered, and Comparative Preparation using the modified coating agent of Comparative Example 4 In the case of Example 6, compared with Preparation Examples 1 and 7 (using Example 5), the hydrophilicity modification effect was excellent, but there was a problem in that the toxicity was rapidly increased.

And, in the case of Comparative Preparation Example 7 using the modified coating agent of Comparative Example 5, when compared with Preparation Examples 1 and 8 (using Example 6), the effect of improving the absorption rate and durable absorption was insufficient. In addition, in the case of Comparative Preparation Example 8 using the modified coating agent of Comparative Example 6, when compared with Preparation Examples 1 and 9 (using Example 7), the absorption rate is not significantly different, but the durability absorption is greatly reduced, There was also the problem of increasing cytotoxicity.

Unlike the present invention without cytotoxicity (Preparation Examples 1 to 9), the existing hydrophilic modification coating agent isopropyl alcohol (Comparative Example 7), a diester and propylene glycol mixture (Comparative Example 8) and CTFA (Comparative Example 9) In the case of the modified coated nonwoven fabric (Comparative Preparation Examples 9 to 11), hydrophilicity was excellent, but it was confirmed that there was a problem with cytotoxicity.

Through the above Examples and Experimental Examples, it was confirmed that the hydrophilic modified coating agent of the present invention efficiently modified hydrophobicity to hydrophilicity, and there was no cytotoxicity. It is expected that, by using the hydrophilic modified coating agent of the present invention, the application range of the industrial nonwoven fabric and/or the nonwoven fabric for hygiene products, which has limited application use, can be greatly expanded.

Claims (10)

15 to 20% by weight of sodium salt, 10 to 16% by weight of maleate, 2 to 8% by weight of phosphate, and a hydrophilic modification coating agent comprising an alcohol ether-based compound in the balance,
The sodium salt is ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethanediyl), sulfobutanedioxane 1,4-bis(2-(C ₁ to C ₃ alkyl) (C ₄ ~ C ₈ containing at least one selected from ester sodium salt, sodium taloate, sodium cocoate and sodium palm kernelate;
The maleate includes bis(2-(C ₁ to C ₃ alkyl) (C ₄ to C ₈ alkyl) maleate,
The phosphate salt is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphoric acid tris(2-ethylhexyl)ester, (Z)-alpha-2-octa Decenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate and poly(oxy-1,2-ethanedinyl), α-dodecyl-ω-hydroxy-, phosphate, potassium salt {Poly( oxy-1,2-ethanediyl), α-dodecyl-ωpotassium salt},
The hydrophilic modified coating agent has a melting point of -3 to 3 ℃,
A solution of the hydrophilic modified coating agent dissolved in water at a concentration of 9 to 12 wt% has a pH of 5.0 to 7.0 at 20°C.
delete delete delete [Claim 2] The non-toxic hydrophilic modification coating agent for non-woven fabrics according to claim 1, wherein the alcohol ether-based compound comprises at least one selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol, and alcohol polyoxyethylene ether. .
[Claim 6] The non-toxic hydrophilic modified coating agent for non-woven fabrics according to claim 1 or 5, wherein the viscosity measured according to ASTM D7042 standard test (20° C.) is 950 to 1,100 mPa.s.
Step 1 of preparing a nonwoven fabric;
A second step of coating a part or all of the non-woven fabric with the non-toxic hydrophilic modified coating agent of claim 6; and
A third step of modifying the nonwoven fabric to be hydrophilic by thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment;
The non-woven fabric of step 1 is a method of manufacturing a non-toxic non-cellular non-woven fabric, characterized in that it contains a hydrophobic fiber.
As a nonwoven fabric in which a part or all of the nonwoven fabric containing hydrophobic fibers is modified with a hydrophilic nonwoven fabric,
A cell non-toxic non-woven fabric comprising 0.1 to 3 wt % of the cell non-toxic hydrophilic modified coating agent for non-woven fabric of claim 6 based on the total weight of the non-woven fabric.
According to claim 8, wherein the hydrophobic fibers are non-toxic cell non-woven fabric, characterized in that the average diameter of 1 μm ~ 50 μm.
[Claim 9] The non-toxic cellulosic nonwoven fabric according to claim 8, wherein the _{cell viability is 70-100% when IC 50 is measured according to the ISO 10993-5 method.}