Resorptive bone ceramic on the basis of tricalcium phosphate

• US 5,141,511 A
• Filed: 02/07/1990
• Issued: 08/25/1992
• Est. Priority Date: 02/08/1989
• Status: Expired due to Fees

• Current Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Original Assignee: Merck Patent GmbH (Merck & Co., Inc.)
• Inventors: Bauer, Gerd
• Primary Examiner(s): Isabella, David
• Assistant Examiner(s): Gualtieri, Gina
• Application Number:
  US07/476,207
• Time in Patent Office: 930 Days
• Field of Search: 623/16, 623/66, 424/423
• US Class Current: 435/325
• CPC Class Codes: A61L 2430/02 for reconstruction of bones; weight-bearing implants
• CPC Class Codes: A61L 27/12 Phosphorus-containing materials, e.g. apatite
• CPC Class Codes: A61L 27/3608 Bone, e.g. demineralised bone matrix [DBM], bone powder
• CPC Class Codes: A61L 27/3691 characterised by physical conditions of the treatment, e.g. applying a compressive force to the composition, pressure cycles, ultrasonic/sonication or microwave treatment, lyophilisation
• CPC Class Codes: A61L 27/58 Materials at least partially resorbable by the body

Abstract

The invention relates to a process for the preparation of a resorptive bone ceramic on the basis of tricalcium phosphate which can be used as a bone replacement material. In the process, natural bone material, freed from the soft tissues, is used as the starting material. The remaining organic substances are removed from this starting material by pyrolysis. The remaining bone material, which consists virtually completely of hydroxyapatite, is subsequently treated with a phosphate carrier and then subjected to a sintering step.

Claims

1. A process for the preparation of a tricalcium phosphate resorptive bone ceramic, wherein natural bone material is separated from soft tissues, and remaining organic substances are removed by pyrolysis, and resulting bone material is subsequently treated with phosphate carrier and then subjected to a sintering step, said process comprising:

removing tissues from natural bone material;

drying the bone material for a predetermined period at an increased temperature of not more than about 150°

C.;

thereafter increasing the temperature to about 550°

C. in a reducing atmosphere or an atmosphere deficient in air;

heating the bone material to a temperature of about 550°

C.-800°

C. under an excess of air, which is in excess of that needed for removal of remaining organic substances by pyrolysis;

cooling the bone material;

treating the bone material with a stoichiometric amount of phosphate carrier to convert hydroxyapatite into tricalcium phosphate; and

sintering the resultant material at a temperature of about 1125°

-1670°

C.

2. A process according to claim 1, wherein said predetermined period of drying is about 12-72 hours at an increased temperature of not more than about 150°

C.

3. A process according to claim 2, wherein, during the drying step, the temperature is gradually increased from ambient temperature to the maximum temperature of about 150°

C.

4. A process according to claim 1, wherein, after the drying step, the temperature is gradually increased to about 550°

C. in a reducing atmosphere or an atmosphere deficient in air.

5. A process according to claim 1, wherein, after the bone material is heated to about 550°

C., the bone material is kept for about 1-24 hours at a temperature of about 550°

C.-800°

C. in an excess of air.

6. A process according to claim 5, wherein, after the bone material is heated to about 550°

C., the temperature is gradually increased up to about 800°

C. in an excess of air.

7. A process according to claim 1, wherein, after pyrolysis and cooling have been effected, the material is treated with an aqueous solution of a phosphate carrier and then dried.

8. A process according to claim 7, wherein said phosphate carrier is from the group consisting of phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate and triammonium phosphate.

9. A process according to claim 7, wherein said phosphate carrier is a phosphorus-rich calcium phosphate of the stoichiometric composition CaO×

2 P₂ O₅.

10. A process according to claim 1, wherein sintering is effected over a period of about 2-6 hours and at a temperature of about 1150°

-1400°

C.

11. A process according to claim 10, wherein the temperature is gradually increased to the sintering temperature.

12. A process according to claim 5, wherein, after the bone material is heated to about 550°

C., the bone material is kept for about 1-24 hours at a temperature of about 750°

-800°

C. in an excess of air.

13. A tricalcium phosphate resorptive bone ceramic produced by the process according to claim 1.

14. A process for preparation of tricalcium phosphate resorptive bone ceramic, comprising:

sintering tricalcium phosphate bone material at a temperature of about 1125°

-1670°

C. wherein said material is derived from natural bone material which has been dried at an increased temperature, for a predetermined period, of not more than about 150°

C., thereafter treated at a further increased temperature of not more than about 550°

C. in a reducing atmosphere or air-deficient atmosphere, heated under an excess of air, which is in excess of that needed for removal of remaining organic substances by pyrolysis, at a temperature of about 550°

C.-800°

C., cooled and then treated with a stoichiometric amount of phosphate carrier to convert the hydroxyapatite of the bone material to tricalcium phosphate.

15. A resorptive bone ceramic comprising tricalcium phosphate:

said ceramic material consisting essentially of sintered tricalcium phosphate which results from treated hydroxyapatite derived from natural bone material and wherein the porous fine structure, characteristic of natural bone, remains intact.