PRODUCTION OF BETA-TRI-CALCIUM PHOSPHATE (BETA-TCP) WITH HIGH PURITY

Abstract

The present invention relates to the method of production of beta-tri-calcium phosphate (-TCP) with high purity and which has an osteoconductive support matrix which can be resorbed and which is bio-compliant when implanted to the defect area and which provides new bone formation in the defect area and which is resorbed while displacing with the newly formed bone in time.

Claims

1. A method to be used in beta-tri-calcium phosphate production, said method is characterized by comprising the steps of: a. Preparing a Ca(OH).sub.2 solution comprising distilled water and Ca(OH).sub.2, b. Mixing the Ca(OH).sub.2 solution at a reaction temperature in a range from 25 to 35 C. c. Adjusting the pH of the Ca(OH).sub.2 solution to the range between 7-9 by using HCl acid, d. Preparing a [(NH.sub.4).sub.2HPO.sub.4] solution comprising distilled water and [(NH.sub.4).sub.2HPO.sub.4], e. Adding the [(NH.sub.4).sub.2HPO.sub.4] solution to the Ca(OH).sub.2 solution, f. Bringing the pH of the combined solution to between 7-9 by using aqueous NH.sub.4OH, g. Leaving the obtained solution to aging for between 8 and 30 hours, h. Preparing a [(NH.sub.4).sub.2SO.sub.4] solution comprising distilled water and [(NH.sub.4).sub.2SO.sub.4], i. Decanting the aged solution and adding the [(NH.sub.4).sub.2SO.sub.4] solution and leaving for aging for 8-30 hours without mixing, j. Filtering the obtained solution and washing with plenty of water such that the pH of the solution becomes between approximately 6 and 8, preferably 7, k. Drying the obtained humid powder in the stove, l. Sintering the dried powder for 1 hour at a temperature between 900 and 1500 C., m. Obtaining the final product by instantaneous cooling of the product at the end of the sintering process.

2. The method according to claim 1, wherein in step e), the [(NH.sub.4).sub.2HPO.sub.4] solution is added to the Ca(OH).sub.2 solution with a flow rate of 3-5 ml/min.

3. The method according to claim 1, wherein step f further comprises mixing the combined solution for 15-30 minutes.

4. The method according to claim 1, wherein in steps g) and i), the solution is left for resting for a duration of 12-28 hours.

5. The method according to claim 1, wherein in step i), the [(NH.sub.4).sub.2SO.sub.4] solution is a 2-4% [(NH.sub.4).sub.2SO.sub.4] solution.

6. The method according to claim 1, wherein in step k), the powder is dried at a temperature between 70 and 100 C.

7. (canceled)

8. (canceled)

9. The method according to claim 4, wherein the solution is aged for 15-24 hours.

10. The method according to claim 5, wherein in step i), the [(NH.sub.4).sub.2SO.sub.4] solution is a 3% [(NH.sub.4).sub.2SO.sub.4] solution.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0040] In this detailed description, the method of production of beta-tri-calcium phosphate (-TCP) with high purity, which has an osteoconductive support matrix which can be resorbed and which is bio-compliant when implanted to the defect area and which provides new bone formation in the defect area and which is resorbed while displacing with the newly formed bone in time, is explained with references to examples without forming any restrictive effect only in order to make the subject more understandable.

[0041] In the production of the subject matter high purity beta-tri-calcium phosphate (-TCP), calcium hydroxide (calcium source) and di-ammonium hydrogen phosphate (phosphate source) are used as the starting substance, and the usage amounts of the starting substances are determined in a stoichiometric manner such that Ca/P proportion is 1.5. The reaction pH is fixed to 7-9 by means of the ammoniac solution and hydro-chloric acid.

[0042] Method of production of beta-tri-calcium phosphate (-TCP) with high purity: [0043] 100 ml distilled water is added onto 0.08 mol Ca(OH).sub.2 and the Ca(OH).sub.2 solution is prepared, [0044] Reaction temperature is brought to 30 C. and mixing is continued, [0045] Reaction pH is adjusted to 7-9 by using HCl acid, [0046] 100 ml distilled water is added onto 0.053 mole [(NH.sub.4).sub.2HPO.sub.4] and by providing complete dissolving, [(NH.sub.4).sub.2HPO.sub.4] solution is prepared, [0047] [(NH.sub.4).sub.2HPO.sub.4] solution is added to the Ca(OH).sub.2 solution such that 3-5 ml is added in a minute (3-5 ml/minute), [0048] The reaction pH is again brought to between 7-9 by means of NH.sub.4OH solution and is mixed for 20 minutes and the reaction is ended at the end of the duration, [0049] The obtained solution is left for aging for 16 hours, [0050] 200 ml distilled water is added onto 6 grams of [(NH.sub.4).sub.2SO.sub.4] and 3% [(NH.sub.4).sub.2SO.sub.4] solution is prepared, [0051] The aged solution is decanted and 3% [(NH.sub.4).sub.2SO.sub.4] solution is added thereon and is again left for aging for 24 hours without mixing, [0052] The obtained solution is filtered by using gooch crucible por: 4 and is washed with plenty of water such that pH is approximately 7, [0053] The obtained humid powder is dried in stove for 24 hours at 90 C., [0054] The dried powder is sintered for 1 hour at 1100 C., [0055] The product is instantaneously cooled at the end of the sintering process.

[0056] The beta-tri-calcium phosphate obtained by means of the subject matter method has white powder form and its purity is crystal particle size is 73.83 nanometers, size distribution is 1-1000 micrometers, density is 2.973 gr/cm3.

[0057] The impurity proportion of beta-tri-calcium phosphate (heavy metals) is such that Pb 0.077, As 0.016, Zn 0.076, Hg 0.015, Cr 0.085, Co 0.07, Ni 0.02, Cd 0.004, Cu 0.13.

[0058] The most important point in tissue engineering is to form response for healing of the bone in the defect region. Another important point is that the bone is structurally integrated with the peripheral bone tissue as a result of re-shaping of the bone. Within this scope, the beta-tri-calcium phosphate powder, synthesized by means of the subject matter method, is chemically held onto the surface of the bone tissue (osteointegration) such that no fibrosis tissue is formed in between, supports new bone formation (osteoconduction), stimulates transformation to osteoblastic phenotype in the peripheral tissue (osteoinduction) and forms the new bone cells in the transferred area of the powder (osteogenesis). Moreover, in order for the beta-tri-calcium phosphate powder synthesized by means of the subject matter method to stimulate the new bone cell, the impurity proportion and the chemical composition are substantially important.

[0059] Beta-tri-calcium phosphate, synthesized by means of the subject matter method, can also be used as absorbent in the food sector, as baking agent, as agent increasing fluidity and as agent preventing agglomeration in foods.