Hydroxylapatite-synthetic resin composites

Claim 2

A process for preparing ceramic hydroxylapatite/polymeric resin composites which comprises coating particulate ceramic hydroxylapatite with a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid by stirring said hydroxylapatite with a solution of said siliceous material, treating the silicated material with an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxysilane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane by adsorption or deposition thereof from a solution of said organosilane in an inert organic solvent, blending the thus treated particulate material with a polymerizable monomer or mixture of polymerizable monomers and polymerizing the blended mixture.

Claim 3

The process according to claim 1 wherein said polymerizable monomers comprise a mixture of bis-GMA, 2,2-bis-propane dimethacrylate and TEGMA, triethylene glycol dimethacrylate.

Claim 4

The process according to claim 2 which comprises blending 70 weight percent of said treated particulate material with a chemically curable 7:3 mixture of said bis-GMA:TEGMA.

Claim 5

The process according to claim 3 wherein said organosilane is γ-methacryloxypropyltrimethoxysilane.

Claim 6

The process according to claim 4 wherein the particles of said ceramic hydroxylapatite have an average size of 5.3 μm.

Claim 7

The process according to claim 5 wherein said ceramic hydroxylapatite particles are activated by etching, prior to silication, by stirring said hydroxylapatite with either aqueous hydrochloric acid or with aqueous hydrochloric acid followed by aqueous magnesium chloride.

Claim 8

A composite which comprises a mixture of particulate ceramic hydroxylapatite and a polymerizable monomer or mixture of polymerizable monomers wherein said ceramic hydroxylapatite particles, prior to mixing with said polymerizable monomer or monomers, contain a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxysilane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.

Claim 9

A composite which comprises a mixture of particulate ceramic hydroxylapatite and a polymerizable monomer or mixture of polymerizable monomers wherein said ceramic hydroxylapatite particles, prior to mixing with said polymerizable monomer or monomers, contain a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxysilane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.

Claim 10

A composite according to claim 7 wherein said polymerizable monomers comprise a mixture of bis-GMA, 2,2-bis-propane dimethacrylate, and TEGMA, triethylene glycol dimethacrylate.

Claim 11

A composite according to claim 8 wherein said composite comprises 70 weight percent of ceramic hydroxylapatite and the balance a chemically-curable 7:3 mixture of said bis-GMA:TEGMA.

Claim 12

A composite according to claim 9 wherein said organosilane is γ-methacryloxypropyltrimethoxysilane.

Claim 13

A composite according to claim 10 wherein the particles of said ceramic hydroxylapatite have an average size of 5.3 μm.

Claim 14

A composite according to claim 11 wherein said ceramic hydroxylapatite particles are activated by etching, prior to silication, by stirring said hydroxylapatite with either aqueous hydrochloric acid or with aqueous hydrochloric acid followed by aqueous magnesium chloride.

Claim 15

A composite which comprises particulate ceramic hydroxylapatite coated with a siliceous material selected from the groyup consisting of sodium silicate, sodium metasilicate and silicic acid and embedded, after treatment with an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxysilane and γ-methacryloxypropyl-tris-(β-methoxethoxy)silane by adsorption or deposition of said organosilane from a solution thereof in an inert organic solvent, by polymerization within a mass of polymeric resin.

Claim 16

A composite which comprises particulate ceramic hydroxylapatite coated with a siliceous material selected from the groyup consisting of sodium silicate, sodium metasilicate and silicic acid and embedded, after treatment with an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxysilane and γ-methacryloxypropyl-tris-(β-methoxethoxy)silane by adsorption or deposition of said organosilane from a solution thereof in an inert organic solvent, by polymerization within a mass of polymeric resin.

Claim 17

A composite according to claim 13 wherein said plymerized resin comprises a mixture of bis-GMA, 2,2-bis-propane dimethacrylate, and TEGMA, triethylene glycol dimethacrylate.

Claim 18

A composite according to claim 14 wherein said composite comprises 70 weight percent of ceramic hydroxylapatite and the balance a chemically cured 7:3 mixture of said bis-GMA:TEGMA.

Claim 19

A composite according to claim 15 wherein said organosilane is γ-methacryloxypropyltrimethoxysilane.

Claim 20

A composite according to claim 16 wherein said ceramic hydroxylapatite particles are activated by etching, prior to silication, by stirring said hydroxylapatite with either aqueous hydrochloric acid or with aqueous hydrochloric acid followed by aqueous magnesium chloride.

Claim 21

A composition adapted for use as a chemically cured dental restorative which comprises two pastes, (A) and (B), for admixture with one another prior to said dental restorative use, paste (A) comprising a mixture of particulate ceramic hydroxylapatite, a polymerizable monomer or mixture of polymerizable monomers and a catalyst for initiation of polymerization and paste (B) comprising a mixture of particulate ceramic hydroxylapatite, a polymeriable monomer or mixture of polymerizable monomers and a polymerization accelerator, wherein said particulate ceramic hydroxylapatite in each of said pastes contains a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxy-silane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.

Claim 22

A composition adapted for use as a chemically cured dental restorative which comprises two pastes, (A) and (B), for admixture with one another prior to said dental restorative use, paste (A) comprising a mixture of particulate ceramic hydroxylapatite, a polymerizable monomer or mixture of polymerizable monomers and a catalyst for initiation of polymerization and paste (B) comprising a mixture of particulate ceramic hydroxylapatite, a polymeriable monomer or mixture of polymerizable monomers and a polymerization accelerator, wherein said particulate ceramic hydroxylapatite in each of said pastes contains a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxy-silane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.

Claim 23

A composition according to claim 18 wherein said polymerizable monomers in each of said pastes (A) and (B) comprises a mixture of bis-GMA, 2,2-bis-propane dimethacrylate, and TEGMA, triethylene glycol dimethacrylate.

Claim 24

A composition according to claim 19 wherein each of said pastes (A) and (B) comprises 70 weight percent of said ceramic hydroxylapatite and the balance a 7:3 mixture of said bis-GMA:TEGMA.

Claim 25

A composition according to claim 20 wherein said organosilane is γ-methacryloxypropyltrimethoxysilane.

Claim 26

A composition according to claim 21 wherein paste (A) contains a 7:3:0.1 mixture of bis-GMA:TEGMA:BPO and paste (B) contains a 7:3:0.05 mixture of bis-GMA:TEGMA:DHET.

Claim 27

A composition according to claim 22 wherein said ceramic hydroxylapatite particles are activated by etching prior to silication by stirring said hydroxylapatite with either aqueous hydrochloric acid or aqueous magnesium chloride or with aqueous hydrochloric acid followed by aqueous magnesium chloride.

Claim 28

A composition adapted for use as an irradiation cured dental restorative which comprises a mixture of particulate ceramic hydroxylapatite, a polymerizable monomer or mixture of polymerizable monomers and a catalyst for initiation of polymerization by exposure to light, wherein said particulate ceramic hydroxylapatite contains a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxy-silane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.

Claim 29

A composition adapted for use as an irradiation cured dental restorative which comprises a mixture of particulate ceramic hydroxylapatite, a polymerizable monomer or mixture of polymerizable monomers and a catalyst for initiation of polymerization by exposure to light, wherein said particulate ceramic hydroxylapatite contains a first coat of a siliceous material selected from the group consisting of sodium silicate, sodium metasilicate and silicic acid and a second coat of an organosilane selected from the group consisting of γ-methacryloxypropyltrimethoxy-silane and γ-methacryloxypropyl-tris-(β-methoxyethoxy) silane.