阅读说明：本技术 一种基于聚（4-羟基丁酸酯）根管填充材料及其制备方法 (Root canal filling material based on poly (4-hydroxybutyrate) and preparation method thereof ) 是由 李志波 袁帅帅 沈勇 阚泽 于 2020-12-23 设计创作，主要内容包括：本发明公开一种基于聚(4-羟基丁酸酯)根管填充材料及其制备方法。本发明以聚(4-羟基丁酸酯)为主相,并加入至少一种表面接枝聚(4-羟基丁酸酯)的无机填料、至少一种对X射线具有阻射作用的化合物和至少一种塑化剂。将上述材料在熔融状态下进行熔融共混制得本发明的根管填充材料。本发明所制备新型树脂填充材料具有优异的生物相容性、稳定性、粘结性和抗渗漏性,为根管治疗填充材料提供了新的选择。(The invention discloses a poly (4-hydroxybutyrate) -based root canal filling material and a preparation method thereof. The invention takes poly (4-hydroxybutyrate) as a main phase, and adds at least one inorganic filler with surface grafted with poly (4-hydroxybutyrate), at least one compound with X-ray radiation resistance and at least one plasticizer. The root canal filling material of the invention is prepared by melting and blending the materials in a melting state. The novel resin filling material prepared by the invention has excellent biocompatibility, stability, cohesiveness and leakage resistance, and provides a new choice for the filling material for root canal therapy.)

1. A root canal filling material based on poly (4-hydroxybutyrate) and a preparation method thereof, wherein the root canal filling material has a main phase of biodegradable thermoplastic polyester-poly (4-hydroxybutyrate) and the mass fraction of the biodegradable thermoplastic polyester-poly (4-hydroxybutyrate) in a mixture is 50-100 wt%.

2. The poly (4-hydroxybutyrate) root canal filling material of claim 1, wherein the poly (4-hydroxybutyrate) has a weight average molecular weight of 10000-100000.

3. The poly (4-hydroxybutyrate) root canal filling material of claim 1, further comprising an inorganic filler with a surface to which is grafted poly (4-hydroxybutyrate) in an amount of up to 50 wt% based on the weight of the mixture.

4. The poly (4-hydroxybutyrate) root canal filling material of claim 3, wherein said inorganic filler with a surface grafted with poly (4-hydroxybutyrate) comprises one or more of hydroxyapatite with a surface grafted with poly (4-hydroxybutyrate), zinc oxide with a surface grafted with poly (4-hydroxybutyrate), tricalcium phosphate with a surface grafted with poly (4-hydroxybutyrate), bioglass with a surface grafted with poly (4-hydroxybutyrate), magnesium oxide with a surface grafted with poly (4-hydroxybutyrate), and white carbon with a surface grafted with poly (4-hydroxybutyrate).

5. The poly (4-hydroxybutyrate) root canal filling material of claim 1, further comprising a compound that blocks X-rays: one or more of barium titanate, bismuth titanate, barium zirconate, calcium tungstate, barium sulfate, zirconium oxide, bismuth oxychloride and tantalum oxide.

6. The poly (4-hydroxybutyrate) root canal filling material of claim 1, further comprising a plasticizer in an amount ranging from 10 to 40 wt% based on the weight of the mixture.

7. The poly (4-hydroxybutyrate) root canal filling of claim 6 wherein the plasticizer is a polyether polyol.

8. The root canal filling material of poly (4-hydroxybutyrate) according to claim 1, wherein said melt blending device is any one of a single screw extruder, a twin screw extruder and an internal mixer.

9. The poly (4-hydroxybutyrate) root canal filling according to claim 1 wherein the melt blending temperature is 70-150 ℃ and the melt blending time is 5-20 minutes.

Technical Field

The invention relates to the field of oral materials, in particular to a poly (4-hydroxybutyrate) -based root canal filling material and a preparation method thereof.

Background

Root canal therapy, also known as endodontic therapy, is the best treatment method for endodontic and periapical diseases. The technology of root canal therapy has improved remarkably in recent years, but the filling material of the root canal, which is an important component thereof, has not been changed remarkably. At present, the solid root canal filling based on the polymer material includes: gutta-percha filling material taking natural eucommia rubber, namely trans-1, 4-polyisoprene as a main phase, a thermoplastic copolymerization modified polymer or graft modified polymer material (CN 101416923B) and a degradable resin filling material Resilon product (US20030113686A1) taking polycaprolactone as a main phase. Since the development of Resilon resin root canal filling materials in 2003, no new root canal filling polymer materials have been developed.

Poly (4-hydroxybutyrate) is a biodegradable medical high molecular polyester approved by the U.S. food and Drug Administration (u.s.fda), and has been used in the fields of surgical sutures, hernia patches and the like. The poly (4-hydroxybutyrate) has a special five-membered oxygen-containing heterocyclic molecular structure, so that the poly (4-hydroxybutyrate) has higher polarity, more excellent biocompatibility, better root canal sealing effect and lower micro-leakage rate compared with polycaprolactone, and the success rate of root canal treatment can be greatly improved. Therefore, the research and development of a novel poly (4-hydroxybutyrate) root canal filling material has important value in the aspects of basic research, clinical application and the like.

Disclosure of Invention

The invention aims to provide better filling material selection for root canal treatment, and provides a root canal filling material based on poly (4-hydroxybutyrate) and a preparation method thereof.

The invention provides a poly (4-hydroxybutyrate) -based root canal filling material and a preparation method thereof, which are realized by the following technical scheme:

the root canal filling material is prepared by uniformly mixing poly (4-hydroxybutyrate), inorganic filler with the surface grafted with poly (4-hydroxybutyrate), compound with the X-ray radiation resistance and plasticizer, and then melting and blending for 5-20 minutes at 70-150 ℃ in a melting state.

The invention adopts the mixture ratio (mass fraction):

the weight average molecular weight of the poly (4-hydroxybutyrate) is 10000-200000.

The inorganic filler with the surface grafted with the poly (4-hydroxybutyrate) is one or more of hydroxyapatite with the surface grafted with the poly (4-hydroxybutyrate), zinc oxide with the surface grafted with the poly (4-hydroxybutyrate), tricalcium phosphate with the surface grafted with the poly (4-hydroxybutyrate), bioglass with the surface grafted with the poly (4-hydroxybutyrate), magnesium oxide with the surface grafted with the poly (4-hydroxybutyrate) and white carbon black with the surface grafted with the poly (4-hydroxybutyrate).

The compound with the X-ray radiation resisting function is one or more of barium titanate, bismuth titanate, barium zirconate, calcium tungstate, barium sulfate, zirconium oxide, bismuth oxychloride and tantalum oxide.

The plasticizer is polyether polyol.

The melt blending is carried out in one of a single screw extruder, a twin screw extruder or an internal mixer.

Compared with the prior art, the invention has the beneficial effects that:

the novel root canal filling material based on poly (4-hydroxybutyrate) prepared by the invention has better biological compatibility, stability, cohesiveness and leakage resistance than Resilon resin filling material. Filling the isolated tooth with a poly (4-hydroxybutyrate) based root canal filling material by using an Epiphony sealant, measuring the bonding strength of the isolated tooth after the isolated tooth is completely cured, wherein the bonding strength of the poly (4-hydroxybutyrate) based root canal filling material can reach 2.01MPa and is higher than 1.50MPa of a Resilon resin filling material; the bacterial micro-leakage at day 30 was 3.85mM/L, less than 4.5mM/L of the Resilon resin packing material.

Detailed Description

The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.

Example 1

The materials are evenly mixed and melted and blended for 10 minutes in an internal mixer at the temperature of 100 ℃ to obtain the root canal filling material. The Epiphony sealer is adopted, the in-vitro tooth is filled with the poly (4-hydroxybutyrate) root canal filling material, the bonding strength is measured after the in-vitro tooth is completely cured, and the bonding strength can reach 1.96 MPa; the bacterial micro-leakage was 4.15mM/L for 30 days. Compared with Resilon resin filling material, the prepared root canal filling material has better stability, cohesiveness and leakage resistance.

Example 2

The materials are evenly mixed and melted and blended for 15 minutes in an internal mixer at the temperature of 120 ℃ to obtain the root canal filling material. The Epiphony sealer is adopted, the isolated tooth is filled with the poly (4-hydroxybutyrate) root canal filling material, the bonding strength is measured after the isolated tooth is completely cured, and the bonding strength can reach 1.86 MPa; the bacterial micro-leakage was 3.96mM/L for 30 days. Compared with Resilon resin filling material, the prepared root canal filling material has better stability, cohesiveness and leakage resistance.

Example 3

The materials are evenly mixed and melted and blended for 8 minutes in an internal mixer at the temperature of 80 ℃ to obtain the root canal filling material. The Epiphony sealer is adopted, the in-vitro tooth is filled with the poly (4-hydroxybutyrate) root canal filling material, the bonding strength is measured after the in-vitro tooth is completely cured, and the bonding strength can reach 1.80 MPa; the bacterial micro-leakage rate for 30 days is. Compared with Resilon resin filling material, the prepared root canal filling material has better stability, cohesiveness and leakage resistance.