Surface-modified in vivo inflammation suppressing material, method for manufacturing same, functional biodegradable composite material applying same, and method for manufacturing functional biodegradable composite material

Abstract

Disclosed are a surface-modified in vivo inflammation suppressing material, a method for manufacturing same, a functional biodegradable composite material applying same, and a method for manufacturing the functional biodegradable composite material. Specifically, provided are an inorganic in vivo inflammation suppressing material with increased hydrophobicity and a method for manufacturing same, and disclosed are a functional biodegradable composite material applying same to a biodegradable polymer with increased hydrophilicity and a method for manufacturing the functional biodegradable composite material.

Description

Surface-modified anti-inflammatory material and method for producing the same, and functional biodegradable composite material using the same and method for producing the same

[0001] The technical idea of ​​the present disclosure relates to a surface-modified anti-inflammatory material and a method for producing the same, and a method for producing a functional biodegradable composite material using the same. Specifically, the present invention provides an inorganic anti-inflammatory material with increased hydrophobicity and a method for producing the same, and relates to a functional biodegradable composite material and a method for producing the same by applying the same to a biodegradable polymer with increased hydrophilicity.

[0002] Conventional metal stents have been proposed as an effective treatment for vascular diseases, but they suffer from the fatal drawback of restenosis and thrombosis after implantation. Drug-eluting stents have been developed to overcome these drawbacks. However, even patients who undergo these stent procedures still face the challenge of lifelong administration of thrombolytics to prevent thrombosis.

[0003] To improve the various shortcomings of conventional stents as described above, biodegradable stents are being actively researched that do not require a separate stent removal procedure as they decompose in accordance with the period of blood vessel regeneration, and can solve the problems of restenosis and thrombosis caused by residual stents.

[0004] However, despite the advantages of these biodegradable stents, there are concerns that stents manufactured from a single biodegradable material may have biased physical properties and may not be suitable for stent manufacturing, and there are concerns that partial inflammation may occur in the body due to acidic monomers formed during the decomposition process of some biodegradable materials.

[0005] In addition, the existing composite material manufacturing process melts the material at high temperatures and extrudes it, so there is no problem when general-purpose plastics such as polyethylene and polypropylene are used, but in the case of biodegradable materials, there is a problem that it is difficult to form a tube when extruding a stent due to a rapid deterioration in physical properties when frequently exposed to heat, and brittleness occurs. To solve these shortcomings, the use of various additives such as stabilizers, antioxidants, and plasticizers is being attempted, but there is a limitation in that the use of additives is greatly restricted because the materials for use in stents are inserted into the body.

[0006] Against this backdrop, there is an urgent need for a functional biodegradable composite material with excellent physical properties and the ability to suppress inflammation in the body, and a method for producing the same.

[0007] The technical idea of ​​the present disclosure is to provide a material that increases the hydrophobicity of hydrophilic magnesium hydroxide as a surface-modified anti-inflammatory material, and a method for producing the same.

[0008] In addition, the technical idea of ​​the present disclosure is to solve a problem by providing a functional biodegradable composite material and a method for manufacturing the same using a surface-modified anti-inflammatory material and a material that increases the hydrophilicity of a hydrophobic biodegradable polymer.

[0009] The problems to be solved by the present disclosure are not limited to the problems mentioned above, and problems to be solved by the present disclosure that are not mentioned can be clearly understood by a person having ordinary knowledge in the technical field to which the present disclosure belongs (“ordinary skilled person”) from the description below.

[0010] In order to achieve the above purpose, a method for manufacturing a surface-modified anti-inflammatory material according to one aspect of the technical idea of ​​the present disclosure is provided.

[0011] As a wet modification method, it may include a step of reacting magnesium hydroxide, ethanol, and a fatty acid modifier; and a step of drying after the reaction is completed to manufacture a surface-modified anti-inflammatory material.

[0012] For example, the fatty acid modifier may be at least one selected from the group consisting of zinc stearate, stearic acid, sodium stearate, and oleic acid.

[0013] For example, the magnesium hydroxide and ethanol may be mixed in a ratio of 1:5 to 1:20 based on their respective weights.

[0014] For example, the fatty acid modifier may be mixed at 1 to 100 phr.

[0015] For example, the above reaction step may be performed at an internal temperature of 70 to 90 degrees Celsius.

[0016] For example, the above reaction step may be performed at 200 to 400 rpm.

[0017] For example, the above reaction step may be performed for 2 to 4 hours.

[0018] For example, the drying step may be performed at 100 to 115 degrees Celsius.

[0019] For example, the drying step may be performed for 12 to 36 hours.

[0020] In addition, according to another aspect of the technical idea of ​​the present disclosure, a surface-modified anti-inflammatory material manufactured by the wet modification method can be provided.

[0021] In addition, a method for manufacturing a surface-modified anti-inflammatory material according to another aspect of the technical idea of ​​the present disclosure is as follows:

[0022] As a dry modification method, it may include a step of first mixing magnesium hydroxide, zirconia balls, and a fatty acid modifier; a step of second mixing using a high-speed grinder after the first mixing is completed; and a step of drying after the mixing is completed to provide a surface-modified anti-inflammatory material.

[0023] For example, the fatty acid modifier may be at least one selected from the group consisting of zinc stearate, stearic acid, and oleic acid.

[0024] For example, the magnesium hydroxide and zirconia balls may be mixed in a ratio of 1:5 to 1:20 based on their respective weights.

[0025] For example, the average diameter of the zirconia ball may be 2 to 20 mm.

[0026] For example, the fatty acid modifier may be mixed at 1 to 100 phr.

[0027] For example, the first mixing step may be performed at 200 to 400 rpm.

[0028] For example, the first mixing step may be performed for 12 to 36 hours.

[0029] For example, the second mixing step may be performed at 200 to 400 rpm.

[0030] For example, the second mixing step may be performed for 30 to 90 seconds, followed by a cooling step for 120 to 240 seconds, repeated 1 to 5 times.

[0031] For example, the drying step may be performed at 100 to 115 degrees Celsius.

[0032] For example, the drying step may be performed for 12 to 36 hours.

[0033] In addition, according to another aspect of the technical idea of ​​the present disclosure, a surface-modified anti-inflammatory material manufactured by the dry modification method can be provided.

[0034] In addition, a method for manufacturing a functional biodegradable composite material according to another aspect of the technical idea of ​​the present disclosure is as follows:

[0035] A step of surface modification of a biodegradable polymer; and a step of mixing and extruding the surface-modified biodegradable polymer and the surface-modified anti-inflammatory material to produce a functional biodegradable composite material.

[0036] The surface modification step of the above biodegradable polymer is:

[0037] A mixing step of heating chloroform and adding PLLA in portions;

[0038] A reaction step of partially adding a polymer modifier after reflux is performed; and

[0039] After the reaction is completed, a second drying step may be included to produce a surface-modified biodegradable polymer.

[0040] For example, the polymer modifier may be at least one selected from the group consisting of vinyltriethoxysilane, (3-aminopropyl)triethoxysilane, (3-glycidoxypropyl)trimethoxysilane, and vinyltriethoxysilane.

[0041] For example, in the above mixing step, chloroform may be stirred at 100 to 400 rpm, and PLLA may be dividedly added at a stirring speed of 250 rpm or more.

[0042] For example, in the above mixing step, PLLA may be divided and injected at a temperature of 50 degrees Celsius or higher.

[0043] For example, in the above mixing step, the polymer modifier may be divided and added at a temperature of 60 degrees Celsius or higher.

[0044] For example, the above reaction step may be performed at 400 to 550 rpm after the polymer modifier is added.

[0045] For example, the above reaction step may be performed for 30 to 90 minutes after the introduction of the polymer modifier.

[0046] For example, the above reaction step may be performed by additionally adding a 10% NaOH aqueous solution.

[0047] For example, the 10% NaOH aqueous solution used in the above reaction step may be added in an amount of 0 to 20 parts by volume based on 400 parts by volume of chloroform.

[0048] For example, the second stage of the drying step may be drying at 40 to 60 degrees Celsius for 12 to 24 hours, and then drying at 100 to 120 degrees Celsius for 4 hours or more.

[0049] For example, the surface-modified anti-inflammatory material used in the extrusion step may be mixed at 0.001 to 20 phr.

[0050] For example, the extrusion step may additionally include PLLA-co-TMC (Poly(L-lactide-co-trimethylene carbonate)).

[0051] For example, PLLA and PLLA-co-TMC used in the extrusion step may be mixed in a ratio of 100:0 to 80:20 based on their respective weights.

[0052] In addition, according to another aspect of the technical idea of ​​the present disclosure, the surface-modified biodegradable polymer can be provided.

[0053] In addition, according to another aspect of the technical idea of ​​the present disclosure, the functional biodegradable composite material can be provided.

[0054] The surface-modified anti-inflammatory material and its manufacturing method according to the technical idea of ​​the present disclosure can provide a functional biodegradable composite material having excellent physical properties and a manufacturing method thereof by increasing the hydrophobicity of hydrophilic magnesium hydroxide and together with a hydrophobic biodegradable polymer.

[0055] In addition, the method for manufacturing a functional biodegradable composite material according to the technical idea of ​​the present disclosure can provide a functional biodegradable composite material and a method for manufacturing the same, which can be extruded even at low temperatures and have excellent physical properties and an anti-inflammatory function, by using a surface-modified anti-inflammatory material and a material that increases the hydrophilicity of a hydrophobic biodegradable polymer.

[0056] The excellent and / or useful effects according to the present disclosure are not limited to the effects of the present disclosure described above, and it should be understood that those skilled in the art will also be able to clearly recognize excellent and / or useful effects of the present disclosure that are not explicitly disclosed in the present disclosure based on the disclosure of the present specification, and that these are intentionally disclosed by the present specification and are clearly included in the scope of the present disclosure.

[0057] FIG. 1 is a flowchart showing a wet manufacturing method of a surface-modified anti-inflammatory material according to an exemplary embodiment of the present disclosure.

[0058] FIG. 2 is a flowchart showing a dry manufacturing method of a surface-modified anti-inflammatory material according to an exemplary embodiment of the present disclosure.

[0059] FIG. 3 is a flowchart showing a method for manufacturing a functional biodegradable composite material according to an exemplary embodiment of the present disclosure.

[0060] FIG. 4 is a diagram showing a process for evaluating the degree of a surface-modified anti-inflammatory material according to an exemplary embodiment of the present disclosure.

[0061] FIG. 5 is a diagram showing the results of observing the hydrophobicity of a surface-modified anti-inflammatory material according to an exemplary embodiment of the present disclosure.

[0062] The following description of the present invention with reference to the drawings is not limited to specific embodiments, and various modifications and embodiments may be made. Furthermore, the following description should be understood to encompass all modifications, equivalents, and alternatives within the spirit and technical scope of the present invention.

[0063] In the following description, terms such as "first," "second," etc. are used to describe various components, and are not intended to limit their meanings. They are used solely to distinguish one component from another. Furthermore, the same reference numbers used throughout this specification represent the same components.

[0064] Unless otherwise stated herein, certain steps or processes may be performed at room temperature. Room temperature may range from 15 to 30 degrees Celsius, and preferably from 20 to 25 degrees Celsius.

[0065] As used herein, singular expressions include plural expressions unless the context clearly dictates otherwise. In addition, terms such as "comprise," "include," or "have" used herein should be interpreted to indicate the presence of a feature, number, step, operation, component, part, or combination thereof described in the specification, and should be understood to not preclude the possibility of the presence or addition of one or more other features, numbers, steps, operations, components, parts, or combinations thereof.

[0066] According to one aspect of the present disclosure, a method for producing a surface-modified anti-inflammatory material can be provided.

[0067] The method for manufacturing the surface-modified anti-inflammatory material may include a wet modification method, a step of reacting magnesium hydroxide, ethanol, and a fatty acid modifier; and a step of drying after the reaction is completed to manufacture the surface-modified anti-inflammatory material.

[0068] When the above wet modification method is used, the surface of magnesium hydroxide can be easily modified using a fatty acid modifier, and by achieving surface modification without using a separate additive, a surface-modified anti-inflammatory material having excellent mixing properties with a biodegradable polymer while maintaining the inherent anti-inflammatory effect of magnesium hydroxide can be provided.

[0069] For example, the fatty acid modifier may be at least one selected from the group consisting of zinc stearate, stearic acid, sodium stearate, and oleic acid.

[0070] For example, the magnesium hydroxide and ethanol may be mixed in a ratio of 1:5 to 1:20 based on their respective weights.

[0071] For example, the fatty acid modifier may be mixed at 1 to 100 phr. In a wet modification method, the fatty acid modifier can achieve excellent modification efficiency when mixed at 1 to 10 phr, more preferably, it can achieve even better modification efficiency when mixed at 1 to 5 phr, and even more preferably, it can be mixed at 3 phr.

[0072] For example, the above reaction step may be performed at an internal temperature of 70 to 90 degrees Celsius.

[0073] For example, the reaction step may be performed at 200 to 400 rpm.

[0074] For example, the above reaction step may be performed for 2 to 4 hours.

[0075] For example, the drying step may be performed at 100 to 115 degrees Celsius.

[0076] For example, the drying step may be performed for 12 to 36 hours.

[0077] In addition, according to another aspect of the present disclosure, a surface-modified anti-inflammatory material manufactured by the wet modification method can be provided.

[0078] In addition, according to another aspect of the present disclosure, a method for producing a surface-modified anti-inflammatory material can be provided.

[0079] The method for manufacturing the surface-modified anti-inflammatory material may include a dry modification method, a first step of mixing magnesium hydroxide, zirconia balls, and a fatty acid modifier; a second step of mixing using a high-speed grinder after the first mixing is completed; and a step of drying after the mixing is completed to provide the surface-modified anti-inflammatory material.

[0080] When the above dry modification method is used, the surface of magnesium hydroxide can be easily modified using a fatty acid modifier, and magnesium hydroxide with the surface modified can be easily provided in a dry environment by using zirconia balls, thereby providing a surface-modified anti-inflammatory material having excellent mixing properties with a biodegradable polymer while maintaining the inherent anti-inflammatory effect of magnesium hydroxide.

[0081] For example, the fatty acid modifier may be at least one selected from the group consisting of zinc stearate, stearic acid, and oleic acid.

[0082] For example, the magnesium hydroxide and zirconia balls may be mixed in a ratio of 1:5 to 1:20 based on their respective weights.

[0083] For example, the average diameter of the zirconia balls may be 2 to 20 mm. The zirconia balls may be mixed and used with zirconia balls of different specifications having different average diameters. For example, zirconia balls having an average diameter of 5 mm may be used, zirconia balls having an average diameter of 10 mm may be used, and zirconia balls having an average diameter of 5 mm and zirconia balls having a diameter of 10 mm may be mixed and used. For example, when zirconia balls having an average diameter of 5 mm and zirconia balls having a diameter of 10 mm are mixed and used, each zirconia ball may exhibit better surface modification characteristics than when mixed and used in a 1:1 ratio by weight.

[0084] For example, the fatty acid modifier may be mixed at 1 to 100 phr. In a dry modification method, the fatty acid modifier can achieve excellent modification efficiency when mixed at 1 to 10 phr, more preferably, when mixed at 3 to 7 phr, even better modification efficiency can be achieved, and even more preferably, when mixed at 5 phr.

[0085] For example, the first mixing step may be performed at 200 to 400 rpm.

[0086] For example, the first mixing step may be performed for 12 to 36 hours.

[0087] For example, the second mixing step may be performed at 200 to 400 rpm.

[0088] For example, the second mixing step may be performed for 30 to 90 seconds, followed by a cooling step for 120 to 240 seconds, repeated 1 to 5 times.

[0089] For example, the drying step may be performed at 100 to 115 degrees Celsius.

[0090] For example, the drying step may be performed for 12 to 36 hours.

[0091] In addition, according to another aspect of the present disclosure, a surface-modified anti-inflammatory material manufactured by the dry modification method can be provided.

[0092] In addition, according to another aspect of the present disclosure, a method for producing a functional biodegradable composite material can be provided.

[0093] The method for manufacturing the functional biodegradable composite material may include a step of surface modification of a biodegradable polymer; and a step of mixing and extruding the surface-modified biodegradable polymer and the surface-modified anti-inflammatory material to manufacture the functional biodegradable composite material.

[0094] The surface modification step of the above biodegradable polymer is:

[0095] A mixing step of heating chloroform and adding PLLA in portions;

[0096] A reaction step of partially adding a polymer modifier after reflux is performed; and

[0097] After the reaction is completed, a second drying step may be included to produce a surface-modified biodegradable polymer.

[0098] For example, the polymer modifier may be at least one selected from the group consisting of vinyltriethoxysilane, (3-aminopropyl)triethoxysilane, (3-glycidoxypropyl)trimethoxysilane, and vinyltriethoxysilane.

[0099] For example, in the above mixing step, chloroform may be stirred at 100 to 400 rpm, and PLLA may be dividedly added at a stirring speed of 250 rpm or more.

[0100] For example, in the above mixing step, PLLA may be divided and injected at a temperature of 50 degrees Celsius or higher.

[0101] For example, in the above mixing step, the polymer modifier may be injected in portions at a temperature of 60 degrees Celsius or higher.

[0102] For example, the reaction step may be performed at 400 to 550 rpm after introducing the polymer modifier.

[0103] For example, the reaction step may be performed for 30 to 90 minutes after the introduction of the polymer modifier.

[0104] For example, the above reaction step may be performed by additionally adding a 10% NaOH aqueous solution.

[0105] For example, the 10% NaOH aqueous solution used in the above reaction step may be added in an amount of 0 to 20 parts by volume based on 400 parts by volume of chloroform.

[0106] For example, the second stage of drying in the above drying step may be drying at 40 to 60 degrees Celsius for 12 to 24 hours, and then drying at 100 to 120 degrees Celsius for 4 hours or more.

[0107] For example, the surface-modified anti-inflammatory material used in the extrusion step may be mixed at 0.001 to 20 phr.

[0108] As an example, the extrusion step may additionally include PLLA-co-TMC (Poly(L-lactide-co-trimethylene carbonate)).

[0109] For example, PLLA and PLLA-co-TMC used in the extrusion step may be mixed in a ratio of 100:0 to 80:20 based on their respective weights.

[0110] Additionally, according to another aspect of the present disclosure, the surface-modified biodegradable polymer can be provided.

[0111] In addition, according to another aspect of the present disclosure, the functional biodegradable composite material can be provided.

[0112] Hereinafter, preferred embodiments of the present invention will be described. However, the following examples are intended only to illustrate the present invention and are not intended to limit the scope of the present invention to the following examples.

[0113] Examples 1 to 15: Preparation of surface-modified anti-inflammatory materials using a wet modification method

[0114] According to the order shown in Fig. 1, 100 g of ethanol was added based on 10 g of magnesium hydroxide, and the reaction was performed for 3 hours under the conditions of an internal temperature of 78 degrees Celsius and 300 rpm. The fatty acid modifier was used in the types and contents shown in Table 1 below. Afterwards, the material for suppressing inflammation in the body of Examples 1 to 15 was prepared by drying overnight at 105 to 110 degrees Celsius for 12 hours.

[0115] Example Modification Fatty acid modifier phr Example 1 Wet zinc stearate 100 Example 2 Wet zinc stearate 5 Example 3 Wet zinc stearate 3 Example 4 Wet zinc stearate 1 Example 5 Wet stearic acid 100 Example 6 Wet stearic acid 5 Example 7 Wet stearic acid 3 Example 8 Wet stearic acid 1 Example 9 Wet sodium stearate 100 Example 10 Wet sodium stearate 5 Example 11 Wet oleic acid 100 Example 12 Wet oleic acid 50 Example 13 Wet oleic acid 10 Example 14 Wet oleic acid 5 Example 15 Wet oleic acid 3

[0116] Examples 16 to 24: Manufacturing of surface-modified anti-inflammatory materials using a dry modification method According to the sequence shown in Figure 2, 100 g of zirconium hydroxide was added based on 10 g of magnesium hydroxide, and the first mixing was performed overnight for 24 hours at 300 rpm. The fatty acid modifier was used in the types and contents shown in Table 1 below. Afterwards, mixing was performed for 1 minute at 5,000 to 20,000 rpm using a stainless steel high-speed grinder, followed by cooling and resting for 3 minutes, and this was repeated 3 times. Afterwards, the mixture was dried overnight at 105 to 110 degrees Celsius for 12 hours to prepare anti-inflammatory materials of Examples 16 to 30.

[0117] Example Modification Fatty acid Modifier phr Zirconia Ball Diameter Example 16 Dry oleic acid 100- Example 17 Dry oleic acid 55 mm, 10 mm Example 18 Dry oleic acid 310 mm Example 19 Dry stearic acid 15 mm, 10 mm Example 20 Dry stearic acid 100 10 mm Example 21 Dry stearic acid 55 mm, 10 mm Example 22 Dry zinc stearate 310 mm Example 23 Dry zinc stearate 15 mm, 10 mm Example 24 Dry zinc stearate 100 10 mm

[0118] Examples 25 to 36: Preparation of surface-modified biodegradable polymers According to the procedure shown in Figure 3, 300 mL of chloroform was added to a 500 mL five-necked flask and heated at 150 rpm. Thereafter, the stirring speed was adjusted to 300 rpm, and after confirming that the temperature of the chloroform reached 50 degrees Celsius or higher, 20 g of PLLA was added in portions. After confirming that the boiling point of approximately 60 degrees Celsius was reached and reflux was performed, the polymer modifiers were added in the types and contents shown in Table 3 below, and 10% NaOH was also added according to the examples.

[0119] Afterwards, the mixture was stirred for 60 minutes at a stirring speed of 400 to 550 rpm, transferred to a tray after the reaction was completed, dried in an oven at 50 degrees Celsius for 18 hours, and then dried at 110 degrees Celsius for more than 4 hours to produce a surface-modified biodegradable polymer.

[0120] Example Modifier phr 10% NaOH (mL) Example 25 STD (PLLA) 00 Example 26 vinyltriethoxysilane 100 Example 27 (3-Aminopropyl)triethoxysilane 100 Example 28 (3-Glycidoxypropyl)trimethoxysilane 100 Example 29 STD (PLLA) 05 Example 30 STD (PLLA) 010 Example 31 vinyltriethoxysilane 105 Example 32 vinyltriethoxysilane 1010 Example 33 (3-Aminopropyl)triethoxysilane 105 Example 34 (3-Aminopropyl)triethoxysilane 1010 Example 35 (3-Glycidoxypropyl)trimethoxysilane 105 Example 36(3-Glycidoxypropyl)trimethoxysilane1010

[0121] Comparative Examples 1 to 3: Application of PLLA / Mg Masterbatch Magnesium hydroxide was mixed with PLLA at 1 phr, 5 phr, and 10 phr, respectively, and storage stability was confirmed under vacuum and room temperature, and then extruded at 150 to 210 degrees Celsius. In all cases, the material deteriorated during the extrusion process and was found to be unsuitable for tube manufacturing.

[0122] Examples 37 to 41: Preparation of functional biodegradable composite materials according to the present disclosure

[0123] Chloroform was added to a 500 ml 5-necked flask and heated at 150 rpm. The stirring speed was then adjusted to 300 rpm, and the surface-modified material was added in portions after confirming that the temperature of the chloroform reached 50 degrees Celsius or higher. After confirming that the boiling point of approximately 60 degrees Celsius was reached and reflux was performed, the mixture was stirred at a stirring speed of 400 to 550 rpm for 60 minutes, and after the reaction was completed, it was transferred to a tray and dried in an oven at 50 degrees Celsius for 18 hours, and then dried at 110 degrees Celsius for more than 4 hours to produce a surface-modified biodegradable composite material. The contents of the components used are shown in Table 4 below. The contents of the components used are shown in Table 4 below.

[0124] Example PLLA (w / w%) PLLA-co-TMC (w / w%) method Mg (OH) 2 (phr) Chloroform (times) Example 37 9010 STD 115 Example 38 9010 1115 Example 39 9010 2115 Example 40 9010 3115 Example 41 9010 4115

[0125] Method 1: Surface modification of magnesium hydroxide (hydrophilic -> hydrophobic)Method 2: Surface modification of biodegradable polymer (hydrophobic -> hydrophilic)

[0126] Method 3: Application of oligomer-magnesium hydroxide

[0127] Method 4: Application of PLLA / Mg Master Batch

[0128] Experimental Example 1: Hydrophobicity Evaluation of Surface-Modified Anti-Inflammation Materials

[0129] The hydrophobicity of the surface-modified anti-inflammatory material was measured by mixing the sample with water, leaving it for 24 hours, and multiplying the weight of the sample suspended in water (g) by the total weight of the sample immersed in water (g) * 100. The process is illustrated in Fig. 4, and the results are presented in Table 5 below.

[0130] Example Hydrophobic Example Hydrophobic Example 1100 Example 13100 Example 2100 Example 14100 Example 3100 Example 15100 Example 410 Example 1611 Example 5100 Example 1749 Example 6100 Example 1811 Example 7100 Example 1961 Example 812 Example 203 Example 9100 Example 21100 Example 100 Example 2242 Example 110 Example 23100 Example 12100 Example 2436

[0131] Referring to Table 5 above, the wet modification method showed the highest efficiency at 3 phr, the dry modification method showed the highest efficiency at 5 phr, the highest efficiency was observed when 5 mm and 10 mm zirconia balls were used in a 1:1 ratio, and it was confirmed that the efficiency was excellent when zinc stearate and stearic acid were used.

[0132] Experimental Example 2: Evaluation of Hydrophilicity of Surface-Modified Biodegradable Polymers

[0133] The hydrophilicity of surface-modified biodegradable polymers was evaluated by dropping a water droplet onto a polymer film and measuring the internal angle of the droplet. A water droplet with an internal angle greater than 90 degrees was considered hydrophobic, while a water droplet with an internal angle less than 90 degrees was considered hydrophilic. The process is illustrated in Figure 5, and the results are presented in Table 6.

[0134] Example Contact Angle Example Contact Angle Example 25107 Example 3170 Example 2686 Example 3267 Example 2772 Example 3378 Example 28109 Example 3465 Example 2962 Example 3570 Example 30106 Example 3690

[0135] In Examples 27, 33, and 34, cracks were observed on the film surface. Referring to Table 6 above, when aminosilane was used, the efficiency was high, but cracks occurred in the film, making it difficult to utilize, and vinylsilane had good film forming characteristics and thus excellent physical properties, while the contact angle was evaluated to be low, confirming that hydrophilicity was improved. In the case of epoxysilane, when it was used alone, the hydrophilic modification effect was low, and when 10% NaOH was used to create basic conditions, the hydrophilic modification effect was confirmed to be excellent. In general, it was confirmed that when basic conditions were created and surface modification was performed, a better hydrophilic surface modification was achieved.

[0136] Experimental Example 3: Performance Evaluation of Functional Biodegradable Composite Materials According to the Present Invention

[0137] The functional biodegradable composite materials according to Examples 37 to 42 were used to manufacture tubes using an extruder at 150°C to 210°C. As a result, in the case of Example 38, it was confirmed that it was possible to manufacture a tube with excellent physical properties, and thus the composite material according to the present disclosure was confirmed to be a composite material of a hydrophobic biodegradable composite material and a hydrophobically modified body inflammation suppressing material, and is a material suitable for tube extrusion.

[0138] Experimental Example 4: Evaluation of the Anti-Inflammatory Effect

[0139] Functional biodegradable composite rods were implanted into female rats weighing 20–30 g, and their anti-inflammatory effects were observed for 12 weeks. As a result, inflammation was observed in rats implanted with the biodegradable composite rods, while no inflammatory response was observed in the biodegradable composite with the modified magnesium hydroxide.

[0140] As described above, exemplary embodiments have been disclosed in the drawings and specifications. While specific terminology has been used to describe embodiments herein, it is intended solely to illustrate the technical concept of the present disclosure and is not intended to limit the scope of the present disclosure as defined in the claims. Therefore, those skilled in the art will understand that various modifications and equivalent embodiments are possible. Therefore, the true scope of technical protection of the present disclosure should be determined by the technical concept of the appended claims.

Claims

1. A method for producing a surface-modified anti-inflammatory material, comprising: a step of reacting magnesium hydroxide, ethanol, and a fatty acid modifier; and a step of drying after the reaction is completed to produce a surface-modified anti-inflammatory material.

2. A method for producing a surface-modified anti-inflammatory material, wherein the fatty acid modifier in the first paragraph is at least one selected from the group consisting of zinc stearate, stearic acid, sodium stearate, and oleic acid.

3. A method for producing a surface-modified anti-inflammatory material, wherein the magnesium hydroxide and ethanol are mixed in a ratio of 1:5 to 1:20 based on their respective weights in the first paragraph.

4. A method for producing a surface-modified anti-inflammatory material, wherein the fatty acid modifier is mixed in an amount of 1 to 100 phr in the first paragraph.

5. A surface-modified anti-inflammatory material manufactured according to the manufacturing method of the surface-modified anti-inflammatory material of paragraph 1.

6. A method for manufacturing a surface-modified anti-inflammatory material, comprising the steps of: first mixing magnesium hydroxide, zirconia balls, and a fatty acid modifier; second mixing using a high-speed grinder after the first mixing is completed; and second mixing using a high-speed grinder after the mixing is completed to provide a surface-modified anti-inflammatory material.

7. A method for producing a surface-modified anti-inflammatory material in accordance with claim 6, wherein the fatty acid modifier is at least one selected from the group consisting of zinc stearate, stearic acid, sodium stearate, and oleic acid.

8. A method for producing a surface-modified anti-inflammatory material, wherein the magnesium hydroxide and the zirconia balls are mixed in a ratio of 1:5 to 1:20 based on their respective weights in the 6th paragraph.

9. A method for manufacturing a surface-modified anti-inflammatory material in accordance with claim 6, wherein the average diameter of the zirconia ball is 2 to 20 mm.

10. A method for producing a surface-modified anti-inflammatory material, wherein the fatty acid modifier is mixed in an amount of 1 to 100 phr in the 6th paragraph.

11. A surface-modified anti-inflammatory material manufactured according to the manufacturing method of the surface-modified anti-inflammatory material of Article 6.

12. A method for manufacturing a functional biodegradable composite material, comprising: a step of surface modification of a biodegradable polymer; and a step of mixing and extruding the surface-modified biodegradable polymer and a surface-modified anti-inflammatory material to manufacture a functional biodegradable composite material. A method for producing a functional biodegradable composite material, wherein the surface modification step of the biodegradable polymer comprises a mixing step of heating chloroform and dividing PLLA into the mixture; a reaction step of dividing a polymer modifier into the mixture after reflux is performed; and a drying step of drying in two stages after the reaction is completed to produce a surface-modified biodegradable polymer.

13. A method for producing a functional biodegradable composite material, wherein the polymer modifier in claim 12 is at least one selected from the group consisting of vinyl triethoxysilane, (3-aminopropyl) triethoxysilane, (3-glycidoxypropyl) trimethoxysilane, and vinyl triethoxysilane.

14. A method for producing a functional biodegradable composite material, wherein the reaction step in paragraph 12 is performed by additionally adding a 10% NaOH aqueous solution.

15. A method for producing a functional biodegradable composite material, wherein the 10% NaOH aqueous solution is added in an amount of 0 to 20 parts by volume based on 400 parts by volume of chloroform in the 14th paragraph.

16. A method for producing a functional biodegradable composite material, wherein the surface-modified anti-inflammatory material used in the extrusion step is mixed at 0.001 to 20 phr in the 12th paragraph.

17. A method for producing a functional biodegradable composite material in claim 12, wherein the extrusion step additionally includes PLLA-co-TMC (Poly(L-lactide-co-trimethylene carbonate)).

18. A method for producing a functional biodegradable composite material, wherein in the 17th paragraph, PLLA and PLLA-co-TMC used in the extrusion step are mixed in a ratio of 100:0 to 80:20 based on their respective weights.

19. A surface-modified biodegradable polymer manufactured according to the surface modification step of the biodegradable polymer according to Article 12.

20. A functional biodegradable composite material manufactured according to the manufacturing method of a functional biodegradable composite material according to Article 12.

Images