KR20240100305A - Dental membrane manufacturing method and dental membrane - Google Patents

Abstract

The present invention includes a mixture preparation step of preparing a mixture by mixing an aqueous alginate solution and an aqueous solution containing a reinforcing agent; A molded product manufacturing step of pouring the mixture into a mold and pressurizing it to produce a molded product; A freeze-drying step of freeze-drying the molded product; A crosslinking step of crosslinking the freeze-dried molded product with an aqueous solution containing a crosslinking agent; A washing step of washing the crosslinked molded product with distilled water; and a drying step of drying the cleaned molded product.

Description

Dental membrane manufacturing method and dental membrane { DENTAL MEMBRANE MANUFACTURING METHOD AND DENTAL MEMBRANE }

The present invention relates to a method of manufacturing a dental membrane and a dental membrane, and is specifically intended for use in guided bone regeneration (GBR), which is widely performed in dentistry. It improves the mechanical strength of a dried porous body, It can reduce softening or deformation due to hydration reactions in the human body, and it addresses the problems of the cost burden of collagen raw materials in collagen membranes, mechanical strength and absorption speed that vary depending on the complex cross-linking method or degree of cross-linking, and residues from chemical cross-linking agents. It relates to a method of manufacturing a dental membrane and a dental membrane with improved mechanical strength and predictable absorption rate through a simple cross-linking method using inexpensive raw materials.

Generally, in dentistry, when bone grafting is required due to alveolar bone loss due to periodontitis, tooth loss due to tooth extraction, or congenital bone deformity, guided bone regeneration (GBR) is performed for a long time to reconstruct the bone in the bone defect. This has been used. For this GBR procedure, the bone defect is filled with bone graft material and then a shielding membrane (membrane) is placed over the bone graft material to block the invasion of epithelial cells that create unwanted fibrous connective tissue and induce desired alveolar bone regeneration. All membranes are used the same way after filling bone defects with bone graft material, but their functions and uses vary depending on the type of membrane material and manufacturing method. As implant surgery has become more popular today, GBR is used together with bone grafting materials to secure the bone quantity and bone quality required for implant placement.

Absorbable collagen products, which are the most widely used among various membrane products for guided bone tissue regeneration (GBR), are usually made of pure type 1 and/or type 3 collagen derived from mammals (cattle, pigs), and if possible, can be stored in the body for a long period of time. It is manufactured to effectively help rebuild the alveolar bone by maintaining its strength and shape while maintaining its dense structure to effectively protect against the penetration of foreign cells or bacteria. In particular, in order to clinically satisfy the basic principles of PASS for guided bone regeneration, collagen decomposition enzyme resistance is improved through sufficient cross-linking during the manufacture of most collagen membranes, which can be maintained for a long time in the body until bone regeneration is completed at the bone graft site. We focus on manufacturing products.

The typical manufacturing process involves dissolving high-purity purified collagen, salt treatment, cross-linking, organic solvent treatment, compression, freeze-drying, and sterilization. However, most absorbable collagen membranes are products designed to decompose after performing a barrier function for a certain period of time, and show very different aspects depending on the cross-linking method or time.

Since most dental bone graft materials are provided in powder or granular form, they are easily scattered from the bone graft area due to bleeding or suction during surgery, and may be damaged when the shield is improperly fixed, the soft tissue valve is manipulated, or the suturing process is not appropriate. Displacement may act as a factor that inhibits bone regeneration.

In addition, attempts are being made to extend the biodegradation period of existing commercially available collagen membranes in the body using chemical/mechanical cross-linking methods, but this method has limitations. In addition, residual cross-linking agent remains are also a problem.

Accordingly, the present inventor delayed the rapid decomposition rate, which is a problem with existing collagen membrane products, and was able to effectively block soft tissue from penetrating into the shielding membrane due to rapid decomposition after implantation for a long period of time, and has a low space maintenance function due to low mechanical strength and rigidity. It can be improved, expensive collagen raw materials can be used as inexpensive materials, the period during which the membrane can function as a shielding film in the body is delayed, the space securing ability is excellent, and the shielding film function period can be predicted while reducing dependence on the use of chemical cross-linking agents. Possible dental membrane manufacturing methods and technology related to dental membranes have been completed.

Korean Patent Publication No. 10-2013-0033826 (2013.04.04.)

One purpose of the invention is to delay the decomposition rate to effectively prevent soft tissue from penetrating into the shielding membrane due to rapid decomposition after transplantation for a long period of time, to improve the low space maintenance function due to low mechanical strength and rigidity, and to improve the function of expensive collagen. A dental membrane manufacturing method and dental technology that can use inexpensive raw materials, has excellent space retention capabilities by delaying the period during which the membrane can function as a shield in the body, and can predict the shield function period while reducing dependence on the use of chemical cross-linking agents. The purpose is to provide a membrane.

The problems to be solved by the present invention are not limited to the problems mentioned above, and other problems not mentioned can be clearly understood by those skilled in the art from the description below.

The present invention according to the first aspect for achieving the above object includes a mixture preparation step of preparing a mixture by mixing an aqueous solution of alginate and an aqueous solution containing a reinforcing agent; A molded product manufacturing step of pouring the mixture into a mold and pressurizing it to produce a molded product; A freeze-drying step of freeze-drying the molded product; A crosslinking step of crosslinking the freeze-dried molded product with an aqueous solution containing a crosslinking agent; A washing step of washing the crosslinked molded product with distilled water; and a drying step of drying the cleaned molded product.

Preferably, the crosslinking agent may be an aqueous solution containing at least one selected from divalent metal ions and trivalent metal ions.

Preferably, the alginate aqueous solution may be characterized as an aqueous solution containing 1 to 3 wt% of alginate powder combined with a Group 1 metal relative to the total 100 wt%.

Preferably, the alginate powder bound to the Group 1 metal may be characterized as alginate powder bound to sodium (Na-alginate powder).

Preferably, the aqueous solution containing the reinforcing agent may be characterized as an aqueous solution of cellulose fibers, which is an aqueous solution containing cellulose fibers.

Preferably, the cellulose fiber aqueous solution may be characterized as an aqueous solution containing 1 to 3 wt% of cellulose relative to the total 100 wt%.

Preferably, the crosslinking agent may be calcium ion.

The present invention according to the second aspect for achieving the above object provides a dental membrane containing alginate, cellulose fibers, and a crosslinking agent.

Preferably, the crosslinking agent may be one or more selected from divalent metal ions and trivalent metal ions.

The dental membrane manufacturing method and dental membrane according to the present invention can effectively block soft tissue from penetrating into the shielding membrane due to rapid decomposition after implantation for a long period of time by delaying the decomposition rate, and improve the low space maintenance function due to low mechanical strength and rigidity. It is possible to use expensive collagen raw materials as inexpensive materials, has excellent space securing ability by delaying the period during which the membrane can function as a shielding membrane in the body, and can predict the period of shielding membrane function while reducing dependence on the use of chemical cross-linking agents. You can.

Figure 1 is a diagram showing a membrane containing μm-sized (about 1 to 100 μm) cellulose fibers according to an embodiment of the present invention.
Figure 2 is a diagram illustrating a membrane comprising nm-sized (about <1 μm or <1000 nm) cellulose fibers according to one embodiment of the present invention.
Figure 3 is a diagram showing a state in which a membrane containing μm-sized (about 1 to 100 μm) cellulose fibers has enough rigidity and strength to be handled with tongs according to an embodiment of the present invention.
Figure 4 is a diagram showing a state in which a membrane containing nm-sized (about 1 to 100 nm) cellulose fibers has enough rigidity and strength to be handled with forceps according to an embodiment of the present invention.

The foregoing and additional aspects are embodied through embodiments described with reference to the accompanying drawings. It is understood that the components of each embodiment can be combined in various ways within the embodiment or with components of other embodiments as long as there is no other mention or contradiction between them. Based on the principle that the inventor can appropriately define the concept of terms in order to explain his or her invention in the best way, the terms used in this specification and claims have meanings that correspond to the description or proposed technical idea. It must be interpreted as a concept.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the attached drawings. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided so that the disclosure will be thorough and complete, and so that the spirit of the invention can be sufficiently conveyed to those skilled in the art. Throughout the specification, the same reference numbers indicate the same components, and components indicated with the same or similar symbols perform the same or similar functions, so descriptions may be omitted. For components with reference symbols whose explanations have been omitted, the content previously described for components with the same or similar symbols can be referred to.

The present invention according to the first aspect for achieving the above object includes a mixture preparation step of preparing a mixture by mixing an aqueous solution of alginate and an aqueous solution containing a reinforcing agent; A molded product manufacturing step of pouring the mixture into a mold and pressurizing it to produce a molded product; A freeze-drying step of freeze-drying the molded product; A crosslinking step of crosslinking the freeze-dried molded product with an aqueous solution containing a crosslinking agent; A washing step of washing the crosslinked molded product with distilled water; and a drying step of drying the cleaned molded article.

By including an alginate aqueous solution in the mixture preparation step, a matrix, which is the basic skeletal structure of the manufactured dental membrane, can be formed.

By including an aqueous solution containing a reinforcing agent in the mixture preparation step, the mechanical strength and rigidity of the manufactured dental membrane can be improved, thereby improving space maintenance.

Specifically, in the molded product manufacturing step, a plate-shaped membrane can be manufactured by pouring a mixture of the desired membrane thickness into a desired mold and applying pressure using a plunger having the inner diameter of the mold. At this time, a membrane with a thickness of 0.5 mm can be manufactured with an error of 0.1 mm.

In the cross-linking step, the cross-linking agent can maintain an attractive force with the electrically negative alginate molecules of the alginate aqueous solution and the reinforcing agent, thereby improving the mechanical strength and rigidity of the manufactured dental membrane and improving space retention.

Through the washing step, cross-linking agents or reinforcing agents that are not involved in cross-linking can be removed through washing. The preferred number of washes may be two.

Preferably, the crosslinking agent may be one or more selected from divalent metal ions and trivalent metal ions.

The cross-linking agent is one or more selected from divalent metal ions and trivalent metal ions, thereby maintaining the attractive force between the alginate molecules of the electrically negative alginate aqueous solution and the reinforcing agent, thereby improving the mechanical strength and rigidity of the manufactured dental membrane. Space maintenance can be improved.

The cross-linking agent may be an aqueous solution containing Ca ions, and calcium chloride (CaCl ₂ ) or calcium acetic acid (Ca(C₂H₃O₂)₂) can be used as a calcium ion source, but in the present invention, an aqueous calcium acetate solution was used.

Preferably, the alginate aqueous solution may be characterized as an aqueous solution containing 1 to 3 wt% of alginate powder combined with a Group 1 metal relative to the total 100 wt%.

The alginate aqueous solution contains 1 to 3 wt% of alginate powder combined with a group 1 metal relative to the total 100 wt%, thereby maintaining an attractive force with the alginate molecules of the electrically negative alginate aqueous solution, and the alginate molecules in the alginate aqueous solution Dispersion can be maintained, and space maintenance can be improved by improving the mechanical strength and rigidity of the manufactured dental membrane.

If the alginate aqueous solution contains alginate powder combined with less than 1 wt% of Group 1 metal compared to the total 100 wt%, it may be difficult to maintain the dispersion of alginate molecules in the alginate aqueous solution, and Group 1 metal greater than 3 wt% If it contains combined alginate powder, it may be inefficient in terms of crosslinking ability.

Preferably, the alginate powder bound to the Group 1 metal may be characterized as alginate powder bound to sodium (Na-alginate powder).

The alginate powder bound to the Group 1 metal is an alginate powder bound to sodium (Na-alginate powder), so it can maintain an attractive force with the alginate molecules and reinforcing agent of the electrically negative alginate aqueous solution, thereby increasing the mechanical strength of the manufactured dental membrane. and rigidity can be improved to improve space maintenance.

Preferably, the aqueous solution containing the reinforcing agent may be characterized as an aqueous solution of cellulose fibers, which is an aqueous solution containing cellulose fibers.

The aqueous solution containing the reinforcing agent is an aqueous solution containing cellulose fibers, and thus can improve the mechanical strength and rigidity of the manufactured dental membrane, thereby improving space retention.

In addition, the cross-linking agent is one or more selected from divalent metal ions and trivalent metal ions, so that it can maintain an attractive force with the alginate molecules of the electrically negative alginate aqueous solution and the cellulose fibers, which are reinforcing agents, and thus improve the mechanical strength and mechanical strength of the manufactured dental membrane. By improving rigidity, space maintenance can be improved.

Preferably, the cellulose fiber aqueous solution may be characterized as an aqueous solution containing 1 to 3 wt% of cellulose relative to the total 100 wt%.

The cellulose fiber aqueous solution is an aqueous solution containing 1 to 3 wt% of cellulose relative to the total 100 wt%, so that it can maintain an attractive force with the cellulose fibers of the electrically negative cellulose fiber aqueous solution, and the cellulose fibers in the cellulose fiber aqueous solution Dispersion can be maintained, and space maintenance can be improved by improving the mechanical strength and rigidity of the manufactured dental membrane.

Preferably, the crosslinking agent may be calcium ion.

Since the cross-linking agent is an aqueous solution of calcium acetate, it can maintain the attractive force between the alginate molecules and the reinforcing agent in the electrically negative alginate aqueous solution, and thus improve the mechanical strength and rigidity of the manufactured dental membrane, thereby improving the space retention ability. .

Hereinafter, other aspects of the present invention for achieving the above object will be described. In the following description of other aspects of the present invention, parts that overlap with the description of the first aspect of the present invention may be viewed as omitted even if no description is made.

The present invention according to the second aspect for achieving the above object provides a dental membrane containing alginate, cellulose fibers, and a crosslinking agent.

By including the alginate, a matrix, which is the basic skeletal structure of the manufactured dental membrane, can be formed.

By including the cellulose fibers, the mechanical strength and rigidity of the manufactured dental membrane can be improved, thereby improving space maintenance.

By including the cross-linking agent, an attractive force can be maintained between the alginate molecules and cellulose fibers of the electrically negative alginate aqueous solution, and thus the mechanical strength and rigidity of the manufactured dental membrane can be improved, thereby improving the space retention ability.

Preferably, the crosslinking agent may be one or more selected from divalent metal ions and trivalent metal ions.

The cross-linking agent is one or more selected from divalent metal ions and trivalent metal ions, so that it can maintain attractive force with the alginate molecules and cellulose fibers of the electrically negative alginate aqueous solution, thereby improving the mechanical strength and rigidity of the manufactured dental membrane. This can improve space maintenance.

Hereinafter, the present invention will be described in more detail through examples. However, the present invention should not be construed as limited by the following examples.

Example 1 - Dental Membrane manufacturing

The dental membrane manufacturing process is as follows.

(1) a mixture preparation step of preparing a mixture by mixing an aqueous alginate solution and an aqueous solution containing a cellulose fiber reinforcement; Pour 1.5 g of alginate powder into 100 cc distilled water and heat to create a 1.5 wt% alginate aqueous solution. To prepare the cellulose aqueous solution, commercial high purity μm (Figure 1) or nm (Figure 2) size 1 wt% liquid cellulose was used, and the alginate aqueous solution and cellulose solution were mixed in a 7:3 ratio.

(2) a molded product manufacturing step of pouring the mixture into a mold and pressurizing it to produce a molded product; Pour the mixture in the amount of the desired membrane thickness into a mold of the desired size or shape and pressurize it using a plunger the size of the inner diameter of the mold to create a smooth, plate-shaped membrane. The amount of mixture is related to the thickness of the final membrane. Here, Figures 1 and 2 are membranes with a thickness of 0.5 mm, and the difference is that in Figure 1, μm-sized cellulose fibers are added, and in Figure 2, nm-sized cellulose fibers are added. In addition, Figures 3 and 4 are 0.2 mm thick membranes, and the difference is that Figure 3 has μm-sized cellulose fibers and Figure 4 has nm-sized cellulose fibers added.

(3) a freeze-drying step of freeze-drying the molded product; In order to maintain the smoothness of the molded foam, it was freeze-dried for 1 day while applying pressure.

(4) a crosslinking step of crosslinking the freeze-dried molded product with an aqueous solution containing a crosslinking agent; In the membrane cross-linking step, an aqueous solution containing one or more selected from divalent or trivalent metal ions can be used as an aqueous solution containing a cross-linking agent (chelating agent), but in the above example, a 4% aqueous calcium acetate solution at pH 7.0 is used. After adjusting to , the molded membrane was immersed and crosslinked at room temperature for 5 minutes.

(5) a washing step of washing the crosslinked molded product with distilled water; Washed twice.

(6) a drying step of drying the washed molded foam; It was slowly dried for 1 day in a dryer at 40°C while applying pressure to maintain smoothness.

In the above, the present invention has been described through embodiments with reference to the accompanying drawings, but it is not limited thereto, and should be interpreted to encompass various modifications that can be easily derived by those skilled in the art. The claims are intended to cover these variations.

Claims (9)

A mixture preparation step of preparing a mixture by mixing an aqueous alginate solution and an aqueous solution containing a reinforcing agent;
A molded product manufacturing step of pouring the mixture into a mold and pressurizing it to produce a molded product;
A freeze-drying step of freeze-drying the molded product;
A crosslinking step of crosslinking the dried molded product with an aqueous solution containing a crosslinking agent;
A washing step of washing the crosslinked molded product with distilled water; and
A drying step of drying the washed molded product;
A method of manufacturing a dental membrane comprising.
According to claim 1,
A method of manufacturing a dental membrane, wherein the crosslinking agent is at least one selected from divalent metal ions and trivalent metal ions. According to claim 1,
A method of manufacturing a dental membrane, characterized in that the alginate aqueous solution is an aqueous solution containing alginate powder combined with 1 to 3 wt% of Group 1 metal relative to the total 100 wt%. According to claim 3,
A method of manufacturing a dental membrane, characterized in that the alginate powder combined with the Group 1 metal is alginate powder combined with sodium (Na-alginate powder). According to claim 1,
A method of manufacturing a dental membrane, characterized in that the aqueous solution containing the reinforcing agent is an aqueous solution of cellulose fibers, which is an aqueous solution containing cellulose fibers. According to claim 5,
A method of manufacturing a dental membrane, characterized in that the cellulose fiber aqueous solution is an aqueous solution containing 1 to 3 wt% of cellulose relative to the total 100 wt%. According to claim 1,
A method of manufacturing a dental membrane, characterized in that the cross-linking agent is calcium ion. Dental membrane containing alginate, cellulose fibers and cross-linking agent. According to claim 8,
A method of manufacturing a dental membrane, wherein the crosslinking agent is at least one selected from divalent metal ions and trivalent metal ions.