Premixed magnesium silicate / calcium silicate-based bioactive material as well as preparation method and application thereof

By premixing magnesium silicate/calcium silicate-based bioactive materials, regulating the hydration process and releasing magnesium ions, the problems of rapid curing and anti-collapse properties of root canal filling materials are solved, achieving a highly efficient antibacterial effect in dental root canal treatment.

CN121489792APending Publication Date: 2026-02-10THE UNIVERSITY OF HONG KONG
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Patent Information

Application Number
CN202511692185.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-18
Publication Date
2026-02-10

AI Technical Summary

Technical Problem

Existing root canal filling materials are insufficient in terms of rapid curing, anti-collapse, and long-lasting antibacterial properties, making it difficult to meet the special needs of dental root canal treatment.

Method used

Premixed magnesium silicate/calcium silicate-based bioactive materials are used. Magnesium silicate regulates the hydration process of calcium silicate, releasing magnesium ions to provide antibacterial effects. Rheology is optimized through liquid phases such as polyethylene glycol, achieving a synergistic improvement in rapid curing, anti-collapse, and antibacterial properties.

Benefits of technology

The material has the ability to cure quickly, is antibacterial, and is resistant to disintegration, meeting the operational requirements of dental root canal treatment and improving surgical efficiency and treatment outcomes.

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Abstract

The invention provides a premixed magnesium silicate / calcium silicate-based bioactive material and a preparation method and application thereof, the premixed magnesium silicate / calcium silicate-based bioactive material is composed of a powder phase and a liquid phase, based on 100 parts by mass of the bioactive material, the powder phase comprises the following components: (a) 20-50 parts of a calcium silicate compound with a chemical formula of nCaO.SiO2, n = 1-3; (b) 1-10 parts of magnesium silicate; (c) 5-25 parts of a filling agent; (d) 10 to 35 parts of an X-ray radiation inhibitor; the particle size of the powder phase ranges from 100 nm to 50 [mu] m, and the particle size of the liquid phase ranges from 100 nm to 50 [mu] m. Compared with the prior art, the premixed magnesium silicate / calcium silicate-based bioactive material provided by the invention has the characteristics of high curing speed, good clinical operability, antibacterial property, collapse resistance, good biocompatibility and the like, and can be used for medical application, especially in the dental restoration field of root canal therapy and the like.
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Description

Technical Field

[0001] This invention belongs to the field of biomedical materials technology, specifically relating to a premixed magnesium silicate / calcium silicate-based bioactive material, its preparation method and application, particularly for dental root canal filling and repair. Background Technology

[0002] Root canal treatment is the primary treatment for pulpitis and periapical periodontitis. Its core steps involve removing infected pulp tissue, disinfecting the root canal system, and tightly filling the root canals with biocompatible materials to prevent reinfection and promote healing of surrounding tissues. The performance of root canal filling materials directly affects the treatment outcome; therefore, their research and development has always been an important direction in oral medicine and materials science.

[0003] Traditional root canal filling systems primarily utilize gutta-percha points in conjunction with sealants. While gutta-percha points offer good plasticity and sealing properties, their lack of bioactivity and insufficient adhesion to the root canal walls can lead to microleakage and secondary infection. Commonly used zinc oxide eugenol (ZOE) sealants, although possessing some antibacterial properties, suffer from low mechanical strength, rapid degradation, and easy solubility in tissue fluid. Furthermore, they fail to stimulate hard tissue regeneration, limiting their application in complex root canal morphologies and cases with open apical foramina.

[0004] In recent years, with the development of biomaterials and nanotechnology, new root canal filling materials have emerged continuously. For example, bioceramic materials (such as iRoot SP and MTA) have become a research hotspot due to their excellent biocompatibility, antibacterial properties, and sealing properties, but their setting time is long and their handling is highly sensitive; antibacterial modified materials (such as gutta-percha points containing chlorhexidine or nanosilver) can enhance the antibacterial effect, but may induce cytotoxicity; while materials that promote bone or induce dentin regeneration (such as bioactive glass or growth factor composite systems) are still in the experimental stage, and their clinical applicability still needs to be verified.

[0005] Several improvements have been proposed in existing patented technologies regarding bioactive filling materials. For example, CN107411976A discloses a premixed calcium silicate / magnesium phosphate biphase composite self-curing root canal filling material. This material utilizes the combination of the rapid acid-base reaction of magnesium phosphate bone cement and the hydration reaction of calcium silicate, which to some extent accelerates the curing speed and improves compressive strength. However, the biphase curing mechanism upon which this system still relies has poor reaction controllability, and precipitation and stratification will occur after long-term storage. Furthermore, excessively high magnesium phosphate content can affect bioactivity, sealing performance, and antibacterial properties. On the other hand, CN120093982A proposes a hemihydrate calcium sulfate-based bone filling material containing magnesium silicate and silicon oxynitride. However, its solid phase composition and water-based system are mainly designed for bone repair, without considering the special needs of root canal treatment for injectability, early hydration and anti-collapse, and ease of clinical operation. It also lacks an effective mechanism for inhibiting common root canal microorganisms.

[0006] Therefore, there is an urgent need to develop a root canal repair material that possesses excellent bioactivity and sealing ability, while simultaneously achieving rapid curing, injectability, anti-collapse properties, and long-lasting antibacterial effects. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of the prior art and provide a premixed magnesium silicate / calcium silicate-based bioactive material with rapid curing characteristics, antibacterial properties and anti-collapse ability. This material is particularly suitable for medical applications such as bone repair and dental fillings.

[0008] Another object of the present invention is to provide a method for preparing the above-mentioned bioactive materials.

[0009] Another object of the present invention is to provide applications of the above-mentioned bioactive materials.

[0010] To achieve the above objectives, the present invention adopts the following technical solution:

[0011] In a first aspect, the present invention provides a premixed magnesium silicate / calcium silicate-based bioactive material, which is composed of a powder phase and a liquid phase. Based on 100 parts by mass of the bioactive material, the powder phase comprises the following components:

[0012] (a) 20 to 50 parts of calcium silicate compound with the chemical formula nCaO•SiO2, where n = 1 to 3;

[0013] (b) 1-10 parts magnesium silicate;

[0014] (c) 5-25 parts of filler;

[0015] (d) 10-35 parts of X-ray blocking agent;

[0016] The particle size of the powder phase is between 100 nm and 50 μm;

[0017] The liquid phase is 15-40 parts.

[0018] In the context of this invention, for the sake of simplicity, "calcium silicate compounds with the chemical formula nCaO•SiO2" will be referred to as "calcium silicate compounds" or "calcium silicate-like compounds" or "calcium silicate class".

[0019] It should be noted that the magnesium silicate (MgSiO3) used in this invention is not a simple replacement or direct transplantation of other magnesium-containing components in existing technologies, nor is it an equivalent replacement of magnesium phosphate. As an indispensable and essential functional component in the system, it addresses complex clinical needs that existing technologies have failed to address, and exhibits the following unique functions:

[0020] Regulating the hydration process of calcium silicate to achieve clinically acceptable rapid curing: Magnesium silicate, through its specific surface activity and ion exchange capacity, effectively regulates the hydration reaction kinetics of calcium silicate phases (such as Ca3SiO5), avoiding the drawbacks of excessively long curing time of traditional calcium silicate materials or short operating windows of MTA-type materials. It achieves curing characteristics that meet both clinical operation time requirements and can quickly establish initial mechanical strength.

[0021] Continuous release of antibacterial magnesium ions, providing long-lasting and biosafe antibacterial effects: Magnesium silicate sustainably and controllably releases magnesium ions (Mg ions) during material hydration and in bodily fluid environments. 2+ Magnesium ions not only significantly inhibit common root canal pathogens (such as Staphylococcus aureus and Escherichia coli), but also produce a synergistic antibacterial effect with the high-pH alkaline environment created by material hydration. This mechanism differs from other technologies that focus on degradation or reactive nitrogen antibacterial mechanisms, providing a more suitable long-lasting antibacterial solution for the root canal environment.

[0022] Improving the rheological properties and anti-collapse properties of the paste: The specific surface characteristics of magnesium silicate micropowder exhibit excellent compatibility and dispersion synergy with the liquid phase, effectively optimizing the rheological properties of the paste and achieving a balance between high injectability and low flowability. Simultaneously, it helps form a more stable aggregate structure in the early stages of curing, enhancing the material's anti-collapse ability in moist root canal environments.

[0023] This invention achieves a comprehensive performance breakthrough that cannot be obtained by a single component through the ingenious design and multi-level synergy of a quaternary system of "magnesium silicate-calcium silicate-filling agent-liquid phase". It achieves a performance balance, especially for the specific needs of root canal treatment, and specifically includes:

[0024] 1. Magnesium silicate and calcium silicate promote each other during hydration. Magnesium silicate accelerates the dissolution of calcium silicate phase and the formation of hydration products, while the alkaline environment generated by calcium silicate hydration promotes the stable release of magnesium ions from magnesium silicate, thereby achieving rapid and controllable curing.

[0025] 2. Mg released from magnesium silicate 2+ Ca produced by the hydration of calcium silicate 2+ and OH - Working together, OH groups provide antibacterial function while... - The alkaline environment created and Ca 2+ PO4 provided by phosphate dissolution 3- Thermodynamic driving force was created for the formation of hydroxyapatite, thereby simultaneously achieving antibacterial and bone / dentin regeneration-promoting bioactivity.

[0026] 3. Synergy between rheology and stability: Liquid phases such as polyethylene glycol (PEG) not only act as wetting agents and plasticizers, but also work together with magnesium silicate and calcium silicate powder particles with specific particle size and surface properties to construct an ideal rheological system through steric effects and viscosity adjustment. This makes the material stable during storage and flows smoothly during injection, ultimately achieving excellent injectability, workability and anti-collapse properties.

[0027] 4. Micro / Nano Size Effect: Powders such as calcium silicate and magnesium silicate have micron or nanometer-scale dimensions. The ultrafine powder creates surface and size effects, which can improve the injectability, manipulability, and anti-collapse properties of the material in this system. Powders with excessively large sizes tend to have poor injectability, manipulability, and anti-collapse properties. On the one hand, larger sizes can lead to needle clogging during use, requiring frequent needle replacements; on the other hand, it can result in poor filling effects, failing to adhere well to the root canal wall or reach the dentinal tubules, leading to poor sealing, leakage, and infection. Furthermore, larger sizes weaken the bond between the powder and liquid phases, making them more prone to disintegration and collapse. Under the size conditions described in this invention, further reducing the powder size would increase the difficulty of the manufacturing process and significantly increase manufacturing costs.

[0028] Therefore, the components in this invention do not function independently within the system, but rather form a closely related and functionally complementary synergistic network. This is the key to the technological breakthrough achieved by this invention and its distinction from existing composition inventions.

[0029] Preferably, the calcium silicate compound is selected from one or more of calcium silicate (CaSiO3), dicalcium silicate (Ca2SiO4), and tricalcium silicate (Ca3SiO5).

[0030] Preferably, the filler is selected from one or more of calcium dihydrogen phosphate, hydroxyapatite, calcium sulfate, lithium carbonate, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, fumed silica, or magnesium stearate.

[0031] Preferably, the X-ray blocking agent is selected from one or more of zirconium oxide, tantalum oxide, and barium sulfate.

[0032] Preferably, the average molecular weight of the polyethylene glycol in the liquid phase is 200 to 10,000.

[0033] Preferably, the viscosity of the silicone oil in the liquid phase is 100~30000 cSt.

[0034] More preferably, the particle size of the powder phase is 100 nm to 50 μm.

[0035] More preferably, the mass ratio of the powder phase to the liquid phase is 1.5:1 to 4:1.

[0036] Secondly, the present invention provides a method for preparing the above-mentioned premixed magnesium silicate / calcium silicate-based bioactive material, comprising the following steps:

[0037] S1: Weigh each component of the powder phase according to the ratio, and mechanically mix them to obtain a uniform powder;

[0038] S2: Mix the powder obtained in step S1 with a liquid phase accounting for 0.1% to 10% of the total liquid phase, and perform stirring and centrifugal degassing treatment in sequence. Then add the remaining liquid phase and mix, and perform stirring and degassing treatment in sequence to finally obtain a uniform paste material.

[0039] Preferably, the mechanical mixing in step S1 is performed at a rotation speed of 100~400 r / min for a time of 10~60 min.

[0040] Preferably, the stirring speed in step S2 is 500~4000 r / min and the time is 2~10 min; the centrifugal degassing speed is 500~4000 r / min and the time is 2~10 min.

[0041] Thirdly, the present invention provides the application of the above-mentioned premixed magnesium silicate / calcium silicate-based bioactive materials in the preparation of medical devices or biomedical materials.

[0042] Preferably, the bioactive material is used as a dental root canal filling and repair material.

[0043] Compared with the prior art, the present invention has the following beneficial effects:

[0044] This invention is the first to introduce magnesium silicate as a component of calcium silicate-based biomaterials, achieving a synergistic improvement in curing speed and antibacterial properties;

[0045] Through the synergistic effect of each component, the material simultaneously possesses three major properties: rapid curing, antibacterial properties, and anti-collapse properties.

[0046] Optimized particle size distribution and preparation process ensure that the material has excellent injection performance;

[0047] The premixed formulation design simplifies clinical procedures and improves surgical efficiency;

[0048] Adjustable curing time meets the needs of different clinical scenarios. Attached Figure Description

[0049] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings, wherein:

[0050] Figure 1 This is a demonstration diagram showing the injectability of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 1 of the present invention;

[0051] Figure 2 This is a flowability demonstration diagram of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 1 of the present invention;

[0052] Figure 3 This is a demonstration diagram showing the solubility test results of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 1 of the present invention.

[0053] Figure 4 This is a diagram demonstrating the anti-collapse properties of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 1 of this invention;

[0054] Figure 5 The diameter distribution of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 2 of this invention was measured according to the flowability test standard at different working times.

[0055] Figure 6 The initial setting time and final setting time of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 2 of this invention;

[0056] Figure 7 This is a comparison image of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 3 of the present invention with a standard wedge-shaped aluminum plate using X-ray photoresistance imaging.

[0057] Figure 8 This is a scanning electron microscope image of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 4 of the present invention;

[0058] Figure 9 The elemental distribution diagram of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 4 of this invention is shown below.

[0059] Figure 10 The pH values ​​of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 5 of this invention after immersion in simulated body fluid for different times;

[0060] Figure 11 This is a diagram demonstrating the antibacterial properties of the magnesium silicate / calcium silicate-based bioactive material prepared in Example 5 of the present invention. Detailed Implementation

[0061] The present invention will be further described in detail below with reference to specific embodiments. The embodiments given are only for illustrating the present invention and are not intended to limit the scope of the present invention.

[0062] This invention develops a premixed bioactive material with excellent performance by optimizing material composition and preparation process. The technical solution of this invention is described in detail below through specific embodiments, but the scope of protection of this invention is not limited thereto.

[0063] Example 1

[0064] Weigh out 2.00 g tricalcium silicate (Ca3SiO5), 0.40 g dicalcium silicate, 0.15 g magnesium silicate (MgSiO3), 0.45 g calcium dihydrogen phosphate, 0.05 g hydroxymethyl cellulose, 1.25 g zirconium oxide (ZrO2), and 1.50 g polyethylene glycol (PEG, average molecular weight 400). First, place the powder in a ball mill jar and ball mill at 130 r / min for 6 h. After ball milling, sieve the powder (particle size range 1-10 μm). The ball-milled powder was mechanically mixed for 10 minutes (200 r / min), then mixed, dispersed, and degassed with 5% liquid (2000 r / min) for 3 minutes. The remaining 95% liquid was then added and mixed, dispersed, and degassed for 3 minutes (2000 r / min). The resulting paste-like premixed bioactive material was transferred to a medical syringe equipped with a cannula needle, thus obtaining a premixed magnesium silicate / calcium silicate-based rapidly curing, antibacterial, and anti-collapse bioactive material.

[0065] After testing, such as Figure 1 As shown, the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material prepared in this embodiment can be smoothly injected through a syringe, with no visible impurities and excellent operability. The inner diameter of the needle is 0.25 mm. Figure 2 This is a flowability demonstration diagram of the premixed magnesium silicate / calcium silicate-based rapid-curing, antibacterial, and anti-collapse bioactive material prepared in this embodiment. The measured diameter is approximately 26 mm, larger than the standard requirement of 17 mm, and the film thickness is 23.33 ± 1.53 μm (less than the standard requirement of 50 μm). Figure 3 As shown, the premixed magnesium silicate / calcium silicate-based rapid-curing, antibacterial, and anti-collapse bioactive material prepared in this embodiment did not disintegrate in the solubility test, with a solubility rate of 2.52% (lower than the specified 3%). Figure 4 As shown, the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material prepared in this embodiment can still maintain its original shape after being immersed in simulated body fluid for 3 hours, and no particulate matter appears, indicating that it has good anti-collapse properties.

[0066] Example 2

[0067] Weigh out 2.00 g tricalcium silicate, 0.40 g dicalcium silicate, 0.15 g magnesium silicate, 0.10 g calcium dihydrogen phosphate, 0.10 g calcium sulfate, 0.05 g sodium carboxymethyl cellulose, 0.05 g lithium carbonate, 0.01 g fumed silica, 1.20 g zirconium oxide, 0.05 g silicone oil (350 cSt), and 1.50 g polyethylene glycol (PEG, average molecular weight 400). First, place the powder in a ball mill jar and ball mill at 130 r / min for 6 h. After ball milling, sieve the powder (particle size range 100 nm–1 μm). The ball-milled powder was mechanically mixed for 10 minutes (200 r / min), then mixed, dispersed, and degassed with 1% liquid (2000 r / min) for 3 minutes. The remaining 99% liquid was then added and mixed, dispersed, and degassed for 3 minutes (2000 r / min). The resulting paste-like premixed bioactive material was transferred to a medical syringe equipped with a cannula needle, thus obtaining a premixed calcium silicate / silicic acid rapid-curing, antibacterial, and anti-collapse bioactive material.

[0068] The diameter distribution diagrams obtained according to the fluidity test standards at different working times are shown below. Figure 5 As shown, the operating time of the premixed magnesium silicate / calcium silicate-based rapid-curing antibacterial material prepared in this embodiment can reach 300 min. Figure 6 As shown, the curing time of the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material was tested using a needle penetration meter. The initial curing time of the bioactive material was approximately 4 hours, and the final curing time was approximately 10 hours.

[0069] Example 3

[0070] Weigh out 2.00 g tricalcium silicate, 0.40 g dicalcium silicate, 0.15 g magnesium silicate, 0.10 g calcium sulfate, 0.05 g sodium carboxymethyl cellulose, 0.05 g lithium carbonate, 0.01 g fumed silica, 0.90 g zirconium oxide, 0.05 g silicone oil (350 cSt), and 1.50 g polyethylene glycol (PEG, average molecular weight 400). First, place the powder in a ball mill jar and ball mill at 130 r / min for 6 h. After ball milling, sieve the powder (particle size range 500 nm-30 μm). The ball-milled powder was mechanically mixed for 10 minutes (200 r / min), then mixed, dispersed, and degassed with 8% of the total liquid phase for 3 minutes (2000 r / min) and 3 minutes (2000 r / min). The remaining 92% of the liquid was then added and mixed, dispersed, and degassed for 3 minutes (2000 r / min) and 3 minutes (2000 r / min). The resulting paste-like premixed bioactive material was transferred to a medical syringe equipped with an injection cannula needle, thus obtaining a premixed magnesium silicate / calcium silicate-based rapidly curing, antibacterial, and anti-collapse bioactive material.

[0071] like Figure 3 As shown in the X-ray radiometric test results, the radiometric effect of the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material obtained in this embodiment is equivalent to the radiometric effect of a 5.3±0.18 mm thick aluminum plate (greater than the equivalent radiometric effect of a 3 mm thick aluminum plate specified in the standard), which indicates that it has excellent X-ray radiometric performance.

[0072] Example 4

[0073] Weigh out 2.00 g tricalcium silicate, 0.40 g dicalcium silicate, 0.15 g magnesium silicate, 0.10 g calcium sulfate, 0.05 g sodium carboxymethyl cellulose, 0.01 g fumed silica, 1.00 g zirconium oxide, 0.05 g silicone oil (350 cSt), and 1.40 g polyethylene glycol (PEG, average molecular weight 400). First, place the powder in a ball mill jar and ball mill at 130 r / min for 6 h. After ball milling, sieve the powder (particle size range 800 nm-2 μm). The ball-milled powder was mechanically mixed for 10 minutes (200 r / min), then mixed, dispersed, and degassed with 0.5% of the total liquid phase for 3 minutes (2000 r / min) and 3 minutes (2000 r / min). The remaining 99.5% of the liquid was then added and mixed, dispersed, and degassed for 3 minutes (2000 r / min) and 3 minutes (2000 r / min). The resulting paste-like premixed bioactive material was transferred to a medical syringe equipped with an injection cannula needle, thus obtaining a premixed magnesium silicate / calcium silicate-based rapidly curing, antibacterial, and anti-collapse bioactive material.

[0074] like Figure 8 As shown in the SEM test results, the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material obtained in this embodiment has small particle size differences among its components, is uniformly distributed, and exhibits no obvious agglomeration. Figure 9 The image shows the elemental distribution of the premixed magnesium silicate / calcium silicate-based rapid curing, antibacterial, and anti-collapse bioactive material obtained in this embodiment. It can be seen that the elements are evenly distributed in this material without agglomeration.

[0075] Example 5

[0076] Weigh out 2.00 g tricalcium silicate, 0.35 g dicalcium silicate, 0.15 g magnesium silicate, 0.10 g calcium sulfate, 0.06 g sodium carboxymethyl cellulose, 0.02 g fumed silica, 0.90 g zirconium oxide, 0.05 g silicone oil (350 cSt), and 1.60 g polyethylene glycol (PEG, average molecular weight 400). First, place the powder in a ball mill jar and ball mill at 130 r / min for 6 h. After ball milling, sieve the powder (particle size range 300 nm-5 μm). The ball-milled powder was mechanically mixed for 10 minutes (200 r / min), then mixed, dispersed, and degassed with 5% liquid (5% of the total liquid phase) for 3 minutes (2000 r / min) and 3 minutes (2000 r / min) respectively. The remaining 95% liquid was then added and mixed, dispersed, and degassed for 3 minutes (2000 r / min) and 3 minutes (2000 r / min) respectively. The resulting paste-like premixed bioactive material was transferred to a medical syringe equipped with an injection cannula needle, thus obtaining a premixed magnesium silicate / calcium silicate-based rapidly curing, antibacterial, and anti-collapse bioactive material.

[0077] After testing, such as Figure 10 As shown, the premixed magnesium silicate / calcium silicate-based rapid-curing antibacterial material prepared in this embodiment increased in pH to approximately 10.5 after being immersed in simulated body fluid for different days, and then stabilized at approximately 12. Figure 11 As shown, the premixed magnesium silicate / calcium silicate-based rapid curing antibacterial material prepared in this embodiment exhibits a clear inhibition zone in the Enterococcus faecalis antibacterial test, indicating that the material has good antibacterial properties.

[0078] The material of this invention is not only applicable to root canal filling, but can also be extended to the following application areas: direct pulp capping and vital pulp preservation treatment, retrograde filling and perforation repair, bone defect repair and bone cement application, trauma orthopedics and spinal fusion, and tissue engineering scaffold materials.

[0079] This invention, through component optimization and process innovation, has successfully developed a premixed bioactive material with rapid curing, excellent antibacterial properties, good handling performance, and biocompatibility. This material overcomes several technical bottlenecks in existing root canal filling materials and has promising clinical application prospects and industrialization value.

[0080] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A premixed magnesium silicate / calcium silicate-based bioactive material, comprising a powder phase and a liquid phase, characterized in that, Based on 100 parts by weight of the bioactive material, the powder phase comprises the following components: (a) 20-50 parts of calcium silicate compound with the chemical formula nCaO·SiO2, where n=1-3; (b) 1-10 parts magnesium silicate; (c) 5-25 parts of filler; (d) 10-35 parts of X-ray blocking agent The particle size of the powder phase is between 100 nm and 50 μm; The liquid phase is 15-40 parts.

2. The bioactive material according to claim 1, wherein, The calcium silicate compound is selected from one or more of calcium silicate, dicalcium silicate, and tricalcium silicate.

3. The bioactive material according to claim 1, wherein, The filler is selected from one or more of the following: calcium dihydrogen phosphate, hydroxyapatite, calcium sulfate, lithium carbonate, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, fumed silica, or magnesium stearate.

4. The bioactive material according to claim 1, wherein, The X-ray blocking agent is selected from one or more of zirconium oxide, tantalum oxide, and barium sulfate.

5. The bioactive material according to claim 1, wherein, The liquid phase includes one or more of polyethylene glycol, silicone oil, and propyl 3-(trimethoxysilyl)methacrylate.

6. The bioactive material according to claim 5, wherein, The average molecular weight of the polyethylene glycol is 200-10000; the viscosity of the silicone oil is 100-30000 cSt.

7. The bioactive material according to claim 1, wherein, The particle size of the powder phase is 100 nm to 50 μm; Preferably, the mass ratio of the powder phase to the liquid phase is 1.5:1 to 4:

1.

8. The method for preparing the premixed magnesium silicate / calcium silicate-based bioactive material according to any one of claims 1 to 7, characterized in that, Includes the following steps: S1. Weigh each component of the ball-milled powder according to the proportion, and mechanically mix them to obtain a uniform powder; S2. The powder obtained in step S1 is mixed with a liquid phase accounting for 0.1% to 10% of the total liquid phase, and the mixture is stirred and centrifuged to remove bubbles. Then the remaining liquid phase is added and mixed, and the mixture is stirred and degassed to obtain a uniform paste material.

9. The preparation method according to claim 8, wherein, The mechanical mixing speed in step S1 is 100~400 r / min, and the time is 10~60 min; Preferably, the stirring speed in step S2 is 500~4000 r / min and the time is 2~10 min; the centrifugal degassing speed is 500~4000 r / min and the time is 2~10 min.

10. The use of the premixed magnesium silicate / calcium silicate-based bioactive material according to any one of claims 1 to 7 in the preparation of medical devices or biomedical materials, preferably, the bioactive material is used as a dental root canal filling and repair material.

Citation Information

Patent Citations

  • Pre-mixed calcium silicate / magnesium phosphate double-phase composite self-solidification root canal filling material and preparation method and application thereof

    CN107411976A