KR101733292B1 - Method for manufacturing titanium hybrid membrane for bone graft comprising hydroxyapatite - Google Patents

Method for manufacturing titanium hybrid membrane for bone graft comprising hydroxyapatite Download PDF

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KR101733292B1
KR101733292B1 KR1020150108357A KR20150108357A KR101733292B1 KR 101733292 B1 KR101733292 B1 KR 101733292B1 KR 1020150108357 A KR1020150108357 A KR 1020150108357A KR 20150108357 A KR20150108357 A KR 20150108357A KR 101733292 B1 KR101733292 B1 KR 101733292B1
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South Korea
Prior art keywords
gel
hydroxyapatite
biodegradable polymer
powder
titanium
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KR1020150108357A
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Korean (ko)
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KR20170014646A (en
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현창용
권태수
정희석
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서울과학기술대학교 산학협력단
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Priority to KR1020150108357A priority Critical patent/KR101733292B1/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/34Macromolecular materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A61L27/44Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
    • A61L27/46Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Veterinary Medicine (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Materials For Medical Uses (AREA)

Abstract

A method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite is provided. The method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite includes the steps of forming a biodegradable polymer gel by gelling a biodegradable polymer, adding a hydroxyapatite powder to the biodegradable polymer gel to form a gel- And applying the gel-powder mixture to a titanium core plate.
The titanium composite shielding film for bone graft containing hydroxyapatite produced by the above-described method can be easily processed by the excellent moldability of the titanium core plate. It is easy to remove after bone regeneration, which can increase the success rate. In addition, the titanium composite shielding film for bone graft containing hydroxyapatite has a low incidence of post-procedure exposure, low risk of infection, and does not perform extensive gingival incision during the second surgery for removal after completion of bone regeneration, Only the site can be removed by incision.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a titanium composite shielding film for bone graft containing hydroxyapatite,

The present invention relates to a method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite, and more particularly, to a method for producing a titanium composite shielding membrane for bone graft incorporating a biodegradable polymer containing hydroxyapatite .

The dental shield is selectively used for successful operation by securing a regeneration space during the bone regeneration period in the alveolar bone defect and preventing the invasion due to the growth of the gum soft tissue in the defect during the period required for bone regeneration.

Conventionally, a method of using an absorbable shielding film using collagen or hyaluronic acid or using a non-absorbable shielding film using titanium or e-PTFE for regeneration of bone structure or regeneration of internal tissue when a bone or joint is deficient in the human body Has been used.

Among these methods, absorptive shielding membranes can not control the degree of absorption in the human body, so they are absorbed before the bone regeneration and cause problems, and inflammation reaction often occurs when absorbed in the human body. In the case of non-absorbable shields, the incidence of infection is low and the risk of infection is high. Secondary surgery is necessary for removal after completion of bone regeneration. Gingival treatment is accompanied by extensive gingival incision.

For this reason, non-absorbable composite shielding membranes with e-PTFE bonded to the core of the titanium sheet material have recently been developed. After bone ingrowth, they are exposed to the soft tissue part of the stapled gum to cause infection. The procedure is very complicated and difficult because of the need for a gingival incision.

In order to solve the above problems, the present invention provides a method for producing a titanium composite shielding membrane for bone graft implantation containing hydroxyapatite having excellent moldability.

The present invention provides a method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite, which is easy to remove during secondary surgery after bone regeneration.

The present invention provides a method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite with less risk of infection.

Other objects of the present invention will become apparent from the following detailed description and the accompanying drawings.

The method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite according to embodiments of the present invention includes the steps of forming a biodegradable polymer gel by gelatinization of a biodegradable polymer and forming a biodegradable polymer gel on the biodegradable polymer gel by adding hydroxyapatite powder To form a gel-powder mixture, and applying the gel-powder mixture to a titanium core plate.

The biodegradable polymer may include polycaprolactone.

The step of forming the biodegradable polymer gel may include mixing the biodegradable polymer and the NaCl aqueous solution into a heating type stirrer, and then rotating the magnetic bar to mix.

The concentration of the NaCl aqueous solution may be 20 wt% to 80 wt%, and the temperature of the heating type stirrer may be 30 ° C to 60 ° C. The rotating speed of the magnetic bar may be 100 rpm to 500 rpm.

The step of forming the gel-powder mixture comprises: milling hydroxyapatite particles to form the hydroxyapatite powder; controlling the particle size of the hydroxyapatite powder; and controlling the particle size of the hydroxyapatite Adding the powder to the biodegradable polymer gel and mixing in a vertical stirrer.

The particle size of the hydroxyapatite powder may be 10 nm to 300 nm.

The mixing in the vertical stirrer may be performed at a rotational speed of 100 rpm to 500 rpm.

Wherein the step of applying the gel-powder mixture to the titanium core plate comprises the steps of disposing the titanium core plate on a glass plate heated to a temperature of 30 캜 to 60 캜, providing the gel-powder mixture on the titanium core plate And a step of horizontally moving the blade while contacting the gel-powder mixture, wherein the interval between the titanium core plate and the blade may be 100 to 500 mu m.

The titanium composite shielding film for bone graft containing hydroxyapatite prepared according to the embodiments of the present invention can be used as a medical shielding film to be applied to patients in medical fields such as dentistry, maxillofacial surgery, plastic surgery, orthopedic surgery, and otorhinolaryngology .

The titanium composite shielding film for bone graft containing hydroxyapatite can be easily processed by the excellent moldability of the titanium core plate. For example, the titanium core plate may be bent or deformed into a desired shape to facilitate use in the missing portion of the tooth. In addition, the biodegradable polymer containing hydroxyapatite is absorbed into the human body, so that it can be easily removed after bone regeneration, thereby increasing the success rate of the operation.

The titanium composite shielding film for bone graft containing hydroxyapatite has a low incidence of exposure after surgery and is less susceptible to infection. In the second operation for removing bone after completion of bone regeneration, It can be removed by incision.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart of a method for manufacturing a titanium composite shielding film for bone graft containing hydroxyapatite according to embodiments of the present invention. FIG.
FIGS. 2A, 2B, and 2C show steps of manufacturing the titanium composite shielding film for bone graft containing hydroxyapatite of FIG. 1, respectively.
3 is a photograph showing a titanium composite shielding film for bone graft containing hydroxyapatite according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail with reference to examples. The objects, features and advantages of the present invention will be easily understood by the following embodiments. The present invention is not limited to the embodiments described herein, but may be embodied in other forms. The embodiments disclosed herein are provided so that the disclosure may be thorough and complete, and that those skilled in the art will be able to convey the spirit of the invention to those skilled in the art. Therefore, the present invention should not be limited by the following examples.

The sizes of the elements in the figures, or the relative sizes between the elements, may be exaggerated somewhat for a clearer understanding of the present invention. In addition, the shape of the elements shown in the drawings may be somewhat modified by variations in the manufacturing process or the like. Accordingly, the embodiments disclosed herein should not be construed as limited to the shapes shown in the drawings unless specifically stated, and should be understood to include some modifications.

1 is a flow chart of a method for manufacturing a titanium composite shielding film for bone graft containing hydroxyapatite according to an embodiment of the present invention.

Referring to FIG. 1, the method for preparing a titanium composite shielding membrane for bone graft containing hydroxyapatite includes the steps of forming a biodegradable polymer gel by gelling a biodegradable polymer (S110), adding hydroxyapatite to the biodegradable polymer gel (S120) adding apatite powder to form a gel-powder mixture (S120), and applying the gel-powder mixture to a titanium core plate (S130).

The biodegradable polymer may include polycaprolactone (PCL). The biodegradable polymer may be in a solid state.

The step of forming the biodegradable polymer gel (S110) may include mixing the biodegradable polymer and the NaCl aqueous solution into a heating type stirrer, and then rotating the magnetic bar to mix the biodegradable polymer gel. The concentration of the NaCl aqueous solution may be 20 wt% to 80 wt%, and the temperature of the heating type stirrer may be 30 ° C to 60 ° C. The rotating speed of the magnetic bar may be 100 rpm to 500 rpm.

The step (S120) of forming the gel-powder mixture comprises the steps of forming the hydroxyapatite powder by pulverizing the hydroxyapatite particles, controlling the particle size of the hydroxyapatite powder, Adding the hydroxyapatite powder to the biodegradable polymer gel, and mixing in a vertical stirrer. The particle size of the hydroxyapatite powder may be 10 nm to 300 nm. The mixing in the vertical stirrer may be performed at a rotational speed of 100 rpm to 500 rpm.

The step (S130) of applying the gel-powder mixture to the titanium core plate comprises the steps of disposing the titanium core plate on a glass plate heated to a temperature of from 30 캜 to 60 캜, applying the gel-powder mixture on the titanium core plate And horizontally moving the blade while contacting the gel-powder mixture, wherein the gap between the titanium core plate and the blade may be between 100 μm and 500 μm.

FIGS. 2A, 2B, and 2C show steps of manufacturing the titanium composite shielding film for bone graft containing hydroxyapatite of FIG. 1, respectively.

Referring to FIGS. 1 and 2A, the biodegradable polymer gel is gelled to form a biodegradable polymer gel 22 (S110). It is possible to gel polycaprolactone as a biodegradable polymer in a solid state. The gelation can be performed by rotating the magnetic bar after placing an aqueous NaCl solution having a concentration of 20 wt% to 80 wt% with the polycaprolactone in a heating type stirrer 21. The temperature of the heating type stirrer 21 may be 30 ° C to 60 ° C, and the rotation speed of the magnetic bar may be 100rpm to 500rpm. Within this temperature range, the solid state polycaprolactone can be prevented from solidifying after being liquefied, and can be liquefied with a homogeneous composition. The caprolactone polymer gel 22 having a desired viscosity can be formed by adjusting the rotation speed of the magnetic bar, the concentration of NaCl, and the temperature of the heating type stirrer 21.

1 and 2B, a hydroxyapatite powder 24 is added to the biodegradable polymer gel 22 to form a gel-powder mixture (S120). The hydroxyapatite powder 24 may be formed by pulverizing hydroxyapatite particles using a pulverization light classifier 23 and then classifying the particles to adjust the particle size of the powder to 10 nm to 300 nm. The gel-powder mixture may be formed by mixing the hydroxyapatite powder 24 having controlled particle size and the caprolactone polymer gel 22 in a vertical mixer. The mixing in the vertical stirrer may be performed at a rotational speed of 100 rpm to 500 rpm. The hydroxyapatite powder (24) can be uniformly distributed in the caprolactone polymer gel (22) by the above mixing. In addition, the hydroxyapatite powder (24) can be uniformly dispersed in the caprolactone polymer gel (22) by adjusting the rotation speed of the stirring bar of the vertical stirrer and the particle size of the hydroxyapatite powder (24).

1 and 2C, the gel-powder mixture 28 is applied to the titanium core plate 27 (S130). A titanium core plate 27 having a thickness regulated is disposed on a glass plate 26 heated to a temperature of 30 to 60 캜 and a gel-powder mixture 28 is provided on the titanium core plate 27. The blades 25 are arranged on the titanium core plate 27 at intervals of 100 μm to 500 μm and horizontally moved while being in contact with the gel-powder mixture 28. The gel-powder mixture 28 can be formed into a film 29 of a constant thickness by the horizontal movement of the blade 25. [ The thickness of the formed film 29 can be adjusted to adjust the distance between the blade 25 and the titanium core plate 27. Thereby, the titanium composite shielding film 30 for bone graft containing hydroxyapatite can be formed.

An actual photograph of the titanium composite shielding film for bone graft containing hydroxyapatite prepared by the above production method is shown in FIG.

Hereinafter, specific embodiments of the present invention have been described. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the disclosed embodiments should be considered in an illustrative rather than a restrictive sense. The scope of the present invention is defined by the appended claims rather than by the foregoing description, and all differences within the scope of equivalents thereof should be construed as being included in the present invention.

21: Heated stirrer
22: caprolactone polymer gel
23: Crushed light classifier
24: Crushed hydroxyapatite powder
25: Blade of blade casting device
26: Glass plate for casting
27: Titanium core plate
28: gel-powder mixture
29: Film formed by blade casting
30: Titanium composite shielding film for bone graft containing hydroxyapatite
31: Photo of Titanium Composite Shield for bone graft containing hydroxyapatite

Claims (9)

Gelling the biodegradable polymer to form a biodegradable polymer gel;
Adding a hydroxyapatite powder to the biodegradable polymer gel to form a gel-powder mixture; And
And applying the gel-powder mixture to a titanium core plate, wherein the hydroxy-apatite-containing gel-powder mixture is applied to a titanium core plate.
The method according to claim 1,
Wherein the biodegradable polymer comprises polycaprolactone. 2. The method of claim 1, wherein the biodegradable polymer comprises polycaprolactone.
The method according to claim 1,
The step of forming the biodegradable polymer gel includes:
And mixing the biodegradable polymer and the NaCl aqueous solution in a heating type agitator and rotating the magnetic bar to mix the hydroxyapatite.
The method of claim 3,
The concentration of the NaCl aqueous solution is 20 wt% to 80 wt%
Wherein the temperature of the heating stirrer is 30 ° C to 60 ° C. The method for manufacturing a titanium composite shielding membrane for bone graft containing hydroxyapatite.
The method of claim 3,
Wherein the rotating speed of the magnetic bar is 100 rpm to 500 rpm. ≪ RTI ID = 0.0 > 11. < / RTI >
The method according to claim 1,
The step of forming the gel-
Pulverizing the hydroxyapatite particles to form the hydroxyapatite powder;
Adjusting the particle size of the hydroxyapatite powder, and
And adding the hydroxyapatite powder having the controlled particle size to the biodegradable polymer gel, and mixing the mixture in a vertical mixer. The method for producing a titanium composite shielding membrane for bone graft containing hydroxyapatite according to claim 1,
The method according to claim 6,
Wherein the hydroxyapatite powder has a particle size of 10nm to 300nm. ≪ RTI ID = 0.0 > 11. < / RTI >
The method according to claim 6,
Wherein the mixing in the vertical stirrer is performed at a rotation speed of 100 rpm to 500 rpm. ≪ RTI ID = 0.0 > 11. < / RTI >
The method according to claim 1,
Wherein the step of applying the gel-powder mixture to the titanium core plate comprises:
Disposing the titanium core plate on a glass plate heated to a temperature of 30 캜 to 60 캜,
Providing the gel-powder mixture on the titanium core plate, and
And moving the blade horizontally while contacting the gel-powder mixture,
Wherein the gap between the titanium core plate and the blade is 100 to 500 占 퐉.
KR1020150108357A 2015-07-30 2015-07-30 Method for manufacturing titanium hybrid membrane for bone graft comprising hydroxyapatite KR101733292B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050158399A1 (en) 2004-01-20 2005-07-21 Yu Hyun S. Method for producing polymeric sol of calcium phosphate compound and method for coating the same on a metal implant
KR100738476B1 (en) 2006-05-08 2007-07-11 주식회사 제노스 Membrane for guided bone regerneration and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050158399A1 (en) 2004-01-20 2005-07-21 Yu Hyun S. Method for producing polymeric sol of calcium phosphate compound and method for coating the same on a metal implant
KR100738476B1 (en) 2006-05-08 2007-07-11 주식회사 제노스 Membrane for guided bone regerneration and preparation method thereof

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