One-part dental adhesive
US-9700491-B2 · Jul 11, 2017 · US
US10493003B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10493003-B2 |
| Application number | US-201715437603-A |
| Country | US |
| Kind code | B2 |
| Filing date | Feb 21, 2017 |
| Priority date | Jul 29, 2014 |
| Publication date | Dec 3, 2019 |
| Grant date | Dec 3, 2019 |
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A composite material including silanated filler and mixed polymerizable monomer, having a stable pasty property which keeps well and has a consistent usability. A composite material containing a silanated filler, a polymerizable monomer, and a polymerization initiator, and may be produced by a process which includes a mixed polymerizable monomer preparing step, a silanation step, a silanated filler preserving step, a composite material preparing step, a composite material preserving step, a composite material filling step, and a small quantity preserving container preserving step.
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The invention claimed is: 1. A method for manufacturing a composite material comprising a filler, a polymerizable monomer, and a polymerization initiator, wherein the method comprises a mixed polymerizable monomer preparing step, a silanation step, a silanated filler preserving step, and a composite material preparing step, wherein: the mixed polymerizable monomer preparing step comprises mixing the polymerizable monomer and the polymerization initiator to prepare a mixed polymerizable monomer, the silanation step comprises preparing a silane treatment liquid by mixing a silane coupling agent and an organic solvent and/or water, charging the silane treatment liquid into the filler in a mixing container, and mixing the filler and the silane treatment liquid at mixing temperature of 1-60° C. for a mixing period of 1 minute-24 hours to prepare a silanated filler, the silanated filler preserving step comprises preserving the silanated filler for a preserving period of 30-600 days to prepare a preserved silanated filler, and the composite material preparing step comprises mixing the mixed polymerizable monomer and the preserved silanated filler to prepare a composite material. 2. The method for manufacturing a composite material of claim 1 , wherein the composite material preparing step comprises performing a kneading step and a defoaming step, wherein the kneading step comprises kneading the mixed polymerizable monomer and the preserved silanated filler at a kneading temperature of 5-60° C. for a kneading period of 5-40 minutes after charging the preserved silanated filler into the mixed polymerizable monomer to prepare a kneaded mixture of the mixed polymerizable monomer and the preserved silanated filler, wherein a ratio of the preserved silanated filler to the mixed polymerizable monomer is 0.1-9 parts by weight of the preserved silanated filler to 1 part by weight of the mixed polymerizable monomer, and the defoaming step comprises defoaming the kneaded mixture of the mixed polymerizable monomer and the preserved silanated filler at 5-200 Torr for a defoaming period of 5-30 minutes. 3. The method for manufacturing a composite material of claim 1 , wherein the composite material preparing step comprises performing a particulate filler kneading step, a particulate filler defoaming step after the particulate filler kneading step, a silanated filler kneading step, and a silanated filler defoaming step after the silanated filler kneading step, wherein the particulate filler kneading step comprises kneading the mixed polymerizable monomer and a particulate filler at a kneading temperature of 5-60° C. for a kneading period of 5-30 minutes after charging the particulate filler into the mixed polymerizable monomer to obtain a kneaded mixture, wherein a ratio of the particulate filler to the mixed polymerizable monomer is 0.01-0.2 parts by weight of the particulate filler to 1 part by weight of the mixed polymerizable monomer, the particulate filler defoaming step comprises defoaming the kneaded mixture of the mixed polymerizable monomer and the particulate filler at 5-200 Torr for a defoaming period of 5-30 minutes to obtain a defoamed kneaded mixture, the silanated filler kneading step comprises charging the preserved silanated filler into the defoamed kneaded mixture of the mixed polymerizable monomer and the particulate filler, and then kneading the defoamed kneaded mixture of the mixed polymerizable monomer, the particulate filler, and the preserved silanated filler at a kneading temperature of 5-60° C. for a kneading period of 5-40 minutes to obtain a kneaded material of the defoamed kneaded mixture of the mixed polymerizable monomer and the particulate filler and the preserved silanated filler, and the silanated filler defoaming step comprises defoaming the kneaded material of the defoamed kneaded mixture of the mixed polymerizable monomer and the particulate filler and the preserved silanated filler at 5-200 Torr for a defoaming period of 5-30 minutes. 4. The method for manufacturing a composite material of claim 1 , wherein a mixing temperature is 1-60° C. and a mixing period is 1 minute-24 hours in the mixed polymerizable monomer preparing step. 5. The method for manufacturing a composite material of claim 1 , further comprising, after the composite material preparing step, a composite material preserving step that comprises preserving 1-8 liters of the composite material prepared in the composite material preparing step at a preserving temperature of 1-25° C. for a preserving period of 10 days-1.5 years. 6. The method for manufacturing a composite material of claim 5 , wherein the composite material preserving step further comprises performing a composite material evaluation step of evaluating a portion of the composite material. 7. The method for manufacturing a composite material of claim 5 , further comprising, after the composite material preserving step, a composite material filling step that comprises filling the composite material extruded from a nozzle of a filling machine into a small quantity preserving container having 1-50 cc volume. 8. The method for manufacturing a composite material of claim 1 , further comprising performing a mixed polymerizable monomer evaluation step of evaluating a portion of the mixed polymerizable monomer. 9. The method for manufacturing a composite material of claim 2 , wherein a mixing temperature is 1-60° C. and a mixing period is 1 minute-24 hours in the mixed polymerizable monomer preparing step. 10. The method for manufacturing a composite material of claim 3 , wherein a mixing temperature is 1-60° C. and a mixing period is 1 minute-24 hours in the mixed polymerizable monomer preparing step. 11. The method for manufacturing a composite material of claim 2 , further comprising, after the composite material preparing step, a composite material preserving step that comprises preserving 1-8 liters of the composite material prepared in the composite material preparing step at a preserving temperature of 1-25° C. for a preserving period of 10 days-1.5 years. 12. The method for manufacturing a composite material of claim 3 , further comprising, after the composite material preparing step, a composite material preserving step that comprises preserving 1-8 liters of the composite material prepared in the composite material preparing step at a preserving temperature of 1-25° C. for a preserving period of 10 days-1.5 years. 13. The method for manufacturing a composite material of claim 4 , further comprising, after the composite material preparing step, a composite material preserving step that comprises preserving 1-8 liters of the composite material prepared in the composite material preparing step at a preserving temperature of 1-25° C. for a preserving period of 10 days-1.5 years. 14. The method for manufacturing a composite material of claim 6 , further comprising, after the composite material preserving step, a composite material filling step that comprises filling the composite material extruded from a nozzle of a filling machine into a small quantity preserving container having 1-50 cc volume.
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