Dental composite material having stable pasty property

Patent metadata

Field	Value
Publication number	US-9603779-B2
Application number	US-201514755549-A
Country	US
Kind code	B2
Filing date	Jun 30, 2015
Priority date	Jul 29, 2014
Publication date	Mar 28, 2017
Grant date	Mar 28, 2017

Abstract

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.

First claim

The invention claimed is:

1. A method for manufacturing a composite material comprising a filler, a polymerizable monomer, and a polymerization initiator, the method comprising 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, wherein:
the mixed polymerizable monomer preparing step comprises charging a polymerization initiator into a polymerizable monomer in a mixing container, and mixing the polymerizable monomer and the polymerization initiator at a mixing temperature of 1-60° C. for a mixing period of 1 minute-24 hours to prepare a mixed polymerizable monomer,
the silanation step comprises preparing a silane treatment liquid containing 1-40% of silane coupling agent, and 99-60% of organic solvent and/or water by mixing the silane coupling agent and the organic solvent and/or water, charging the silane treatment liquid into the filler in the mixing container at the ratio of 1-15 parts by weight of the silane coupling agent based on 1 part by weight the filler, 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,
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 silanated filler at a kneading temperature of 5-60° C. for a kneading period of 5-40 minutes after charging the silanated filler into the mixed polymerizable monomer to prepare a kneaded mixture of the mixed polymerizable monomer and the silanated filler, wherein a ratio of the silanated filler to the mixed polymerizable monomer is 0.1-9 parts by weight of the 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 silanated filler at 5-200 Torr for a defoaming period of 5-30 minutes to prepare a composite material,

the composite material preserving step 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,
the composite material filling step comprises filling the composite material extruded from a nozzle of a filling machine into a small quantity preserving container having 1-50 cc of volume, and
the small quantity preserving container preserving step comprises preserving the composite material in the small quantity preserving container at a preserving temperature of 1-40° C. for a preserving period of 50 days-5 years.

2. The method for manufacturing a composite material of claim 1 , wherein the composite material preserving step comprises a composite material evaluation step of evaluating a portion of the composite material.

3. The method for manufacturing a composite material of claim 1 , wherein
the method further comprises, between the silanated filler preserving step and the kneading step of the composite material preparing step,
a particulate filler kneading step that comprises a step of 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, 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, and
a particulate filler defoaming step after the particulate filler kneading step comprises defoaming the mixed polymerizable monomer and the particulate filler at 5-200 Torr for a defoaming period of 5-30 minutes,

wherein the mixture obtained from the particulate filler kneading step and the particulate filler defoaming step is utilized in the subsequent composite material preparing step,
wherein the particulate filler is kneaded with the mixed polymerizable monomer and the silanated filler in the kneading step,
wherein the particulate filler is defoamed with the mixed polymerizable monomer and the silanated filler in the defoaming step, and
wherein the composite material prepared in the defoaming step comprises the particulate filler, the silanated filler, a polymerizable monomer, and a polymerization initiator.

4. A method comprising:
mixing a polymerizable monomer and a polymerization initiator at a mixing temperature of 1-60° C. for a mixing period of 1 minute-24 hours to prepare a mixed polymerizable monomer,
preparing a silane treatment liquid containing 1-40% of silane coupling agent, and 99-60% of organic solvent and/or water by mixing the silane coupling agent and the organic solvent and/or water, charging the silane treatment liquid into a filler in a mixing container at the ratio of 1-15 parts by weight of the silane coupling agent based on 1 part by weight of the filler, 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,
preserving the silanated filler in a silanated filler preserving container for 30-600 days,
kneading the mixed polymerizable monomer and the silanated filler at 5-60° C. for 5-40 minutes to prepare a kneaded mixture of the mixed polymerizable monomer and the silanated filler, wherein a ratio of the silanated filler to the mixed polymerizable monomer is 0.1-9 parts by weight of the silanated filler to 1 part by weight of the mixed polymerizable monomer,
defoaming the kneaded mixture of the mixed polymerizable monomer and the silanated filler at 5-200 Torr for 5-30 minutes to prepare a composite material,
preserving 1-8 liters of the composite material in a composite material preserving container at 1-25° C. for 10 days-1.5 years,
transferring a portion of the composite material to a container having 1-50 cc of volume, and
preserving the transferred composite material in the container having 1-50 cc of volume at 1-40° C. for 50 days-5 years.

5. The method of claim 4 , wherein
the method further comprises, between preserving the silanated filler and kneading the mixed polymerizable monomer and the silanated filler,
kneading the mixed polymerizable monomer and a particulate filler at 5-60° C. for 5-30 minutes to prepare a kneaded mixture of the mixed polymerizable monomer and the silanated filler, 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, and
defoaming the kneaded mixture of the mixed polymerizable monomer and the particulate filler at 5-200 Torr for 5-30 minutes,

wherein the mixture obtained from the defoaming of the kneaded mixture of the mixed polymerizable monomer and the particulate filler is utilized in the subsequent kneading.

Assignees

• Shofu Inc

Inventors

• Kadobayashi Yusei
• Shigezawa Masako

Classifications

• A61K6/62

  Photochemical radical initiators · CPC title

• A61K6/80

  Preparations for artificial teeth, for filling teeth or for capping teeth · CPC title

• A61K6/60 Primary

  comprising organic or organo-metallic additives · CPC title

• A61K6/77

  Glass · CPC title

• A61K6/887

  Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds · CPC title