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Publication Number
US-9206080-B2
Publication Date
2015-12-08
Expiration Date
Abstract
Non-aqueous hydraulic cement compositions comprise a non-aqueous mixture of a powder composition and a non-aqueous water-miscible liquid. In one embodiment, powder composition is a Brushite or Monetite-forming calcium phosphate powder composition. In another embodiment, the powder composition comprises porous β-tricalcium phosphate (β-TCP) granules and at least one additional calcium phosphate powder. In another embodiment, the powder composition comprises calcium silicate powder. In a further embodiment, the powder composition comprises calcium aluminate powder. In another embodiment, the powder composition is a cement composition and comprises nanopowders having a grain size of less than 1 micron. Hardened cements are formed from such hydraulic cement compositions, and methods of producing hardened cements, kits, and articles of manufacture employ such hydraulic cement compositions.
Core Innovation
The invention relates to a non-aqueous, hydraulic cement composition in which a non-hydrated cement-forming powder is combined with a non-aqueous water-miscible liquid so that a hardened cement forms upon hydration on contact with a water source. The non-hydrated powder is a Brushite- or Monetite-cement forming powder composition having a setting pH of less than 6.0 and comprising β-tricalcium phosphate powder together with at least one additional calcium phosphate powder selected from monocalcium phosphate monohydrate and anhydrous monocalcium phosphate, including mixtures thereof.
The composition further specifies powder particle size limits, with particles having a size below 300 micrometers and above 20 micrometers, and defines the powder-to-liquid proportions. In particular, the powder composition is mixed with a non-aqueous water-miscible liquid comprising glycerol, with the weight to volume ratio of the powder composition to the non-aqueous water-miscible liquid being about 2.5:1 to about 5:1 in the described embodiments.
Additional formulation aspects include controlling the relative amounts of β-TCP and the additional calcium phosphate, including a 1:1 molar ratio, or a weight ratio of β-TCP powder to the additional calcium phosphate powder in a range about 1:3 to about 3:1. The document also describes contacting the hydraulic cement composition with a hydration liquid or vapor to produce a hardened cement with controlled setting/working time, and states that optional additives can be included for stability, biological response, and additional properties.
Claims Coverage
The independent claims are clm-00001, clm-00024, and clm-00027. Across these claims, the inventive coverage centers on a non-aqueous hydraulic cement composition defined by a non-hydrated Brushite- or Monetite-cement forming powder, specific particle size limits, and mixing with a non-aqueous water-miscible liquid comprising glycerol under specified powder-to-liquid weight-to-volume ratios, with additional quantitative constraints on component ratios for particular claim sets.
Non-aqueous hydraulic cement composition with non-hydrated Brushite- or Monetite powder and glycerol liquid
A non-aqueous, hydraulic cement composition comprising a non-hydrated Brushite- or Monetite-cement forming powder composition having a setting pH of less than 6.0 and comprising β-tricalcium phosphate powder and at least one additional calcium phosphate powder selected from monocalcium phosphate monohydrate, anhydrous monocalcium phosphate, and mixtures thereof, and a non-aqueous water-miscible liquid, wherein the powder composition comprises particles having a size below 300 micrometers and above 20 micrometers, with the non-aqueous water-miscible liquid comprising glycerol.
Specific β-TCP to additional calcium phosphate weight ratio and powder-to-glycerol ratio
A non-aqueous, hydraulic cement composition comprising the non-hydrated Brushite- or Monetite-cement forming powder composition having setting pH less than 6.0 and comprising β-tricalcium phosphate powder and at least one additional calcium phosphate powder selected from monocalcium phosphate monohydrate, anhydrous monocalcium phosphate, and mixtures thereof, wherein the weight ratio of β-TCP powder to the additional calcium phosphate powder is in a range about 1:3 to about 3:1, and wherein the powder composition comprises particles having a size below 300 micrometers and above 20 micrometers; and non-aqueous water-miscible liquid comprising glycerol, wherein the weight to volume ratio of the powder composition to the non-aqueous water-miscible liquid is in a range of about 2.5:1 to about 5:1.
Monetite embodiment with 1:1 molar ratio and powder-to-glycerol ratio
A non-aqueous, hydraulic cement composition comprising a non-hydrated Monetite-cement forming powder composition having a setting pH of less than 6.0 and comprising β-tricalcium phosphate powder and at least one additional calcium phosphate powder selected from monocalcium phosphate monohydrate, anhydrous monocalcium phosphate, and mixtures thereof, wherein the β-TCP powder and the additional calcium phosphate powder are included in a 1:1 molar ratio, and wherein the powder composition comprises particles having a size below 300 micrometers and above 20 micrometers, and a non-aqueous water-miscible liquid comprising glycerol, wherein the weight to volume ratio of the powder composition to the non-aqueous water-miscible liquid is in a range of about 2.5:1 to about 5:1.
Collectively, the independent claims cover a non-aqueous hydraulic cement composition in which a non-hydrated Brushite- or Monetite-cement forming powder is combined with a glycerol-containing non-aqueous water-miscible liquid under a specified powder-to-liquid weight-to-volume ratio range, with additional quantitative constraints on β-TCP to additional calcium phosphate ratio in the Brushite/Monetite and Monetite embodiments.
Stated Advantages
Improved handling.
Reduced waste.
Controlled setting/working time.
Documented Applications
Root-canal filling material.
Hardened cement formed by contacting the hydraulic cement composition with a hydration liquid or vapor, including use in vertebra defect model and in vivo immunologic response as described in examples.
Drug release where tested, including tobramycin.
Radio-opacity measurement where tested, including for radiopaque agents.
Kit/syringe/vacuum packaging formats as described in the document.
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