Siriphannon Punnama, Monvisade Pathavuth
Department of Chemistry, Faculty of Science, King Mongkut's Institute of Technology Ladkrabang, Chalongkrung Road, Ladkrabang, Bangkok, Thailand.
J Biomater Sci Polym Ed. 2008;19(7):925-36. doi: 10.1163/156856208784613569.
Hydroxyapatite/poly(ethylene adipate) (HAp/PEA) composites were prepared by in situ ring-opening polymerization of cyclic oligo(ethylene adipate) (C-OEA) within the porous HAp templates. HAp was firstly prepared by a co-precipitation method using calcium hydroxide and phosphoric acid and then shaped as a rectangular porous template. PEA precursor was synthesized by bulk polymerization of dimethyl adipate and ethylene glycol in the presence of tetraisopropyl orthotitanate. C-OEA was obtained by cyclo-depolymerization of the PEA precursor under high dilution condition using dibutyl tinoxide as a catalyst. The HAp/PEA composites were prepared by immersing the porous HAp templates in the mixture solution of C-OEA and dibutyl tinoxide catalyst overnight and ring-opening polymerizing at 180, 200 and 220 degrees C for 24 h. The ring-opening polymerized PEA formed as a thin film coating on the surface of porous HAp template. The HAp/PEA composites contained PEA in the range of 20-26 wt%. The weight-average molecular weights of ring-opening polymerized PEA were in the range of 3800-4450 g/mol. Compressive strength of the HAp/PEA composite was significantly increased from 25 MPa in the porous HAp template to 140 MPa in the composite.
通过在多孔羟基磷灰石(HAp)模板内使环状低聚己二酸乙二酯(C - OEA)进行原位开环聚合制备了羟基磷灰石/聚己二酸乙二酯(HAp/PEA)复合材料。首先采用氢氧化钙和磷酸通过共沉淀法制备HAp,然后将其成型为矩形多孔模板。在原钛酸四异丙酯存在下,通过己二酸二甲酯和乙二醇的本体聚合合成PEA前体。使用二丁基氧化锡作为催化剂,在高稀释条件下通过PEA前体的环解聚获得C - OEA。通过将多孔HAp模板在C - OEA和二丁基氧化锡催化剂的混合溶液中浸泡过夜,并在180、200和220℃下开环聚合24小时来制备HAp/PEA复合材料。开环聚合的PEA在多孔HAp模板表面形成薄膜涂层。HAp/PEA复合材料中PEA的含量在20 - 26 wt%范围内。开环聚合的PEA的重均分子量在3800 - 4450 g/mol范围内。HAp/PEA复合材料的抗压强度从多孔HAp模板中的25 MPa显著提高到复合材料中的140 MPa。