A Study on the Optimum Conditions for Preparation of Calcium hydrogenphosphate Dihydrate by Box-Wilson Experimental Design

Box-Wilson 실험계획에 의한 연마용 인산일수소칼슘의 최적 제조조건 추구 및 안정화

An abrasive, calcium hydrogen phosphate dihydrate (DCPD), was synthesized in a Box-wilson experimental design by reactions between phosphoric acid and milk of lime, and calcium chloride and sodium phosphate solutions, and stabilized with TSPP and TMP. The optimum conditions for preparation of DCPD from phosphoric acid with milk of lime were such as; reaction temp.; $51.9^{\circ}C$, conc. of lime; 25.9%, conc. of phosphoric acd; 77.9%, drying temp.; $60.2^{\circ}C$ and final pH; 6.46. The physico-chemical and pharmaceutical properties of DCPD were showed as follows: glycerin absorption value(68 ml/100g), whiteness(99.5%), particle size(10.9 nm), pH(7.8), and set test(pass). XRD and SEM of DCPD indicated a monoclinic system crystallographically. $N_2$ adsorption isotherm curve by BET showed non porous type II form. The micromeritic parameters of DCPD showed that surface area was $3.27{\sim}4.6\;cm^{2}/g$ and pore volume, pore area and pore radius were negligible. The rheogram of the toothpaste containing DCPD showed pseudoplastic flow with yield value of 321, and thixotropic behavior forming hysteresis loop. These results meet the requirements as abrasive standard, and sythesized DCPD is expected as a good dental abrasive such as a high quality grade in practice.