Organic-inorganic nano composite resin and preparation method thereof

Abstract

The invention relates to organic-inorganic nano composite resin and a preparation method thereof, belonging to the technical field of biomedical high-molecular materials. The organic-inorganic nano composite resin is characterized in that polyfunctional reactive nano monomer, i.e. polyhedral oligosilsesquioxane (POSS) is added on the basis of organic matrixes and inorganic fillers. The preparation method comprises the steps of adding the POSS into the resin matrixes, placing in a constant-temperature oven, fully dissolving the POSS in the resin matrixes and even agitating; adding an initiator system and evenly agitating; adding the inorganic fillers which are subject to surface silanization treatment, fully and evenly agitating in a vacuum agitator and removing air bubbles to obtain nano composite resin paste. By adding the POSS into dental composite resin, polymerization shrinkage can be obviously reduced, the mechanical property of the composite resin is comprehensively improved, the micro-leakage performance and the biocompatibility are good and the application prospect in the field of oral rehabilitation is wide. Besides, the preparation process is simple, the cost is lower and the popularization value and the application value are great.

Description

technical field

[0001] The invention belongs to the technical field of biomedical polymer materials, and in particular relates to a dental composite resin containing organic-inorganic nanometer functional monomer POSS and a preparation process thereof. Background technique

[0002] Dental composite resin is a kind of restorative material composed of organic monomer system, inorganic filler and initiator system. It is attached to the surface of the tooth through bonding technology, and achieves the purpose of restoration through plastic building, curing, shaping, and polishing. It has been more and more widely used in the field of dental restoration. Most of the existing dental composite resins are light-curing resins induced by free radicals. This resin is characterized by a large volume shrinkage during the curing process, and micro-leakage between the tooth and the restoration is prone to occur, which in turn causes secondary caries. . Polymerization shrinkage can also c...

Examples

specific Embodiment approach 1

[0017] Embodiment 1: The composite resin in this embodiment is composed of resin matrix (mass ratio 14.8~39.8%) and inorganic filler (mass ratio 60~85%), and a functional monomer—organic- Inorganic polyfunctional reactive nano-monomer POSS, the mass ratio is 0.2~15%.

[0018] In this embodiment:

[0019] 1. The polymerizable monomer system includes resin monomer / diluent, and its mass ratio is 40~70:30~60, for example, the mass ratio is 50 / 50 or 70 / 30;

[0020] 2. The initiator system (for the initial polymerization reaction) includes photoinitiator / organic amine activator (mass ratio 1:1), and the mass ratio is 0.2~0.8% of the resin matrix;

[0021] 3. The mass ratio of the photoinitiator in the resin matrix is ​​0.2~0.8%. The photoinitiator includes camphorquinone (CQ), benzil, 4, 4'-dimethoxybenzil, α-diketone and Phenylpropane, Trimethylbenzoyl, Diphenylphosphine Oxide, 2,4-Dimethicone, and photosensitive pigments (tetrabromofluorescein / amine, riboflavin, floral pigment);...

specific Embodiment approach 2

[0028] Embodiment 2: The composite resin in this embodiment includes a resin matrix and an inorganic filler, which are mixed in a mass ratio of 40%:60%. The mass ratio of functional monomer POSS-methacrylate is 0.2~15%, which partially replaces the resin matrix, and is added to the composite resin and mixed evenly.

[0029] The specific steps are:

[0030] 1. The resin monomer Bis-GMA is placed in a constant temperature drying oven at 70°C and left to stand for 40 minutes to greatly reduce the viscosity and meet the mixing needs;

[0031] 2. Put the resin monomer Bis-GMA and the diluent TEGDMA into a light-proof container with a mass fraction of 40% and 60% respectively, and stir magnetically at room temperature for 30 minutes;

[0032] 3. Add the functional monomer—organic-inorganic multifunctional reactive nanomonomer multifunctional methacrylic-based multifaceted oligomeric oligomeric silsesquioxane POSS-methacrylate into the container, partially replace the resin matrix, ...

specific Embodiment approach 3

[0037] Embodiment 3: The composite resin in this embodiment includes a resin matrix and an inorganic filler, which are mixed in a mass ratio of 40%:60%. The resin matrix includes a resin monomer system and an initiator system, wherein the resin monomer system Bis-GMA / TEGDMA is mixed at a mass ratio of 49.5%:49.5%, and then the initiator system CQ / DMAEMA with a mass ratio of 0.5%:0.5% is added. The inorganic filler is barium glass powder (average diameter 0.8μm) with silanized surface. The functional monomer POSS-methacrylate is 0%, 2%, 5%, 10% and 15% by weight, respectively, and partially replaces the resin matrix, and is added to the composite resin and mixed evenly.

[0038] The specific ratio of nanocomposite resin is shown in Table 1.

[0039] Table 1 Components of dental nanocomposite resins (wt%)

[0040]

[0041] According to the relevant regulations in ISO3521, the density ρ of the material before and after light curing is measured by the pycnometer method, and t...

technical field

[0001] The invention belongs to the technical field of biomedical polymer materials, and in particular relates to a dental composite resin containing organic-inorganic nanometer functional monomer POSS and a preparation process thereof. Background technique

[0002] Dental composite resin is a kind of restorative material composed of organic monomer system, inorganic filler and initiator system. It is attached to the surface of the tooth through bonding technology, and achieves the purpose of restoration through plastic building, curing, shaping, and polishing. It has been more and more widely used in the field of dental restoration. Most of the existing dental composite resins are light-curing resins induced by free radicals. This resin is characterized by a large volume shrinkage during the curing process, and micro-leakage between the tooth and the restoration is prone to occur, which in turn causes secondary caries. . Polymerization shrinkage can also c...

Examples

specific Embodiment approach 1

[0017] Embodiment 1: The composite resin in this embodiment is composed of resin matrix (mass ratio 14.8~39.8%) and inorganic filler (mass ratio 60~85%), and a functional monomer—organic- Inorganic polyfunctional reactive nano-monomer POSS, the mass ratio is 0.2~15%.

[0018] In this embodiment:

[0019] 1. The polymerizable monomer system includes resin monomer / diluent, and its mass ratio is 40~70:30~60, for example, the mass ratio is 50 / 50 or 70 / 30;

[0020] 2. The initiator system (for the initial polymerization reaction) includes photoinitiator / organic amine activator (mass ratio 1:1), and the mass ratio is 0.2~0.8% of the resin matrix;

[0021] 3. The mass ratio of the photoinitiator in the resin matrix is ​​0.2~0.8%. The photoinitiator includes camphorquinone (CQ), benzil, 4, 4'-dimethoxybenzil, α-diketone and Phenylpropane, Trimethylbenzoyl, Diphenylphosphine Oxide, 2,4-Dimethicone, and photosensitive pigments (tetrabromofluorescein / amine, riboflavin, floral pigment);...

specific Embodiment approach 2

[0028] Embodiment 2: The composite resin in this embodiment includes a resin matrix and an inorganic filler, which are mixed in a mass ratio of 40%:60%. The mass ratio of functional monomer POSS-methacrylate is 0.2~15%, which partially replaces the resin matrix, and is added to the composite resin and mixed evenly.

[0029] The specific steps are:

[0030] 1. The resin monomer Bis-GMA is placed in a constant temperature drying oven at 70°C and left to stand for 40 minutes to greatly reduce the viscosity and meet the mixing needs;

[0031] 2. Put the resin monomer Bis-GMA and the diluent TEGDMA into a light-proof container with a mass fraction of 40% and 60% respectively, and stir magnetically at room temperature for 30 minutes;

[0032] 3. Add the functional monomer—organic-inorganic multifunctional reactive nanomonomer multifunctional methacrylic-based multifaceted oligomeric oligomeric silsesquioxane POSS-methacrylate into the container, partially replace the resin matrix, ...

specific Embodiment approach 3

[0037] Embodiment 3: The composite resin in this embodiment includes a resin matrix and an inorganic filler, which are mixed in a mass ratio of 40%:60%. The resin matrix includes a resin monomer system and an initiator system, wherein the resin monomer system Bis-GMA / TEGDMA is mixed at a mass ratio of 49.5%:49.5%, and then the initiator system CQ / DMAEMA with a mass ratio of 0.5%:0.5% is added. The inorganic filler is barium glass powder (average diameter 0.8μm) with silanized surface. The functional monomer POSS-methacrylate is 0%, 2%, 5%, 10% and 15% by weight, respectively, and partially replaces the resin matrix, and is added to the composite resin and mixed evenly.

[0038] The specific ratio of nanocomposite resin is shown in Table 1.

[0039] Table 1 Components of dental nanocomposite resins (wt%)

[0040]

[0041] According to the relevant regulations in ISO3521, the density ρ of the material before and after light curing is measured by the pycnometer method, and t...

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