PEEK/NANO-HA COMPOSITES FOR SLS AND PREPARATION METHODS THEREOF

• US 20180155496A1
• Filed: 02/02/2018
• Published: 06/07/2018
• Est. Priority Date: 09/02/2015
• Status: Active Grant

• Current Assignee: Guangdong Silver Age Sci & Tech Co., Ltd.
• Original Assignee: Guangdong Silver Age Sci & Tech Co., Ltd.
• Inventors: YAN, Chunze, SHI, Yusheng, FU, Yi, SHI, Yunsong, PAN, Teng, WANG, Yan, WEI, Qingsong, LIU, Jie
• Granted Patent: US 10,106,651 B2
• Time in Patent Office: Days
• CPC Class Codes: B22F 10/28 Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
• CPC Class Codes: B29B 13/06 by drying B29B13/08 takes precedence ; drying moulded articles or half products B29C37/0092
• CPC Class Codes: B29B 13/10 by grinding, e.g. by triturating; by sieving; by filtering
• CPC Class Codes: B29C 64/153 using layers of powder being selectively joined, e.g. by selective laser sintering or melting
• CPC Class Codes: B29K 2071/00 Use of polyethers , e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof, as moulding material
• CPC Class Codes: C08G 2650/40 containing ketone groups, e.g. polyarylethylketones, PEEK or PEK
• CPC Class Codes: C08G 65/4012 Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
• CPC Class Codes: C08G 65/46 Post-polymerisation treatment, e.g. recovery, purification, drying
• CPC Class Codes: C08K 2003/325 Calcium, strontium or barium phosphate
• CPC Class Codes: C08K 2201/005 Additives being defined by their particle size in general
• CPC Class Codes: C08K 2201/011 Nanostructured additives
• CPC Class Codes: C08K 3/32 Phosphorus-containing compounds
• CPC Class Codes: C08L 61/16 of ketones with phenols
• CPC Class Codes: C08L 71/00 Compositions of polyethers obtained by reactions forming an ether link in the main chain of polyacetals C08L59/00; of epoxy resins C08L63/00; of polythioether-ethers C08L81/02; of polyether-sulfones C08L81/06; Compositions of derivatives of such polymers
• CPC Class Codes: Y02P 10/25 Process efficiency

Abstract

The present invention discloses polyetheretherketone/nano-hydroxyapatite (PEEK/NANO-HA) composites for selective laser sintering (SLS), and a preparation method thereof. The method for preparing the composites comprises steps of: selecting PEEK having a particle size of 10-100 μm, and an aqueous solution of reaction precursor 1 and an aqueous solution of reaction precursor 2, uniformly dispersing the PEEK in the aqueous solution of reaction precursor 1, adding the aqueous solution of reaction precursor 2 dropwise in the mixed solution of the aqueous solution of reaction precursor 1 and the PEEK while stirring to adjust pH of the mixed solution to 10-12, and continuously reacting or 24-48 hours. The composites obtained by the preparation method of the present invention have the advantages of good biocompatibility, homogeneous morphology and good fluidity, and are advantageous to the powdering and shaping process during SLS.

Claims

1. A method for preparing Polyetheretherketone/Nano-hydroxyapatite (PEEK/NANO-HA) composites for Selective Laser Sintering (SLS), comprising steps of:

(1) selecting PEEK having a particle size of 10-100 μ

m;

(2) adding the PEEK in the step (1) to an aqueous solution of reaction precursor 1 so that the PEEK is uniformly dispersed in the aqueous solution;

(3) stirring the mixed solution obtained in the step (2), adding an aqueous solution of reaction precursor 2 dropwise in the mixed solution to adjust pH to 10-12, and reacting for 24-48 hours while stirring; and

(4) at last, vacuum filtering the mixed solution, and washing, drying and grinding the filter cake to eventually obtain the PEEK/NANO-HA composites,

wherein the reaction precursor 1 is a precursor solution containing calcium ions, the reaction precursor 2 is a precursor solution containing phosphate ions, and the reaction precursor 1 and the reaction precursor 2 are dosed such that the mole ratio of Ca/P is 1.67-2.0.

2. The preparation method according to claim 1, wherein, in the step (1), the PEEK has a particle size of 20-70 μ

m.

3. The preparation method according to claim 1, wherein the concentration of the aqueous solution of reaction precursor 1 is 0.5-1.0 mol/L, and the concentration of the aqueous solution of reaction precursor 2 is 1.0-2.0 mol/L.

4. The preparation method according to claim 1, wherein the reaction precursor 1 is Ca(OH)₂ or Ca(NO₃)₂, and the reaction precursor 2 is H₃PO₄ or (NH₄)₂HPO₄.

5. The preparation method according to claim 4, wherein, in the step (2), the reaction precursor 1 is Ca(OH)₂, and in the step (3), the reaction precursor 2 is H₃PO₄.

6. The preparation method according to claim 4, wherein, in the step (2), the reaction precursor 1 is Ca(NO₃)₂.4H₂O, and in the step (3), the reaction precursor 2 is (NH₄)₂HPO₄.

7. PEEK/NANO-HA composites prepared by the method for preparing PEEK/NANO-HA composites for selective laser sintering (SLS) according to claim 1.

8. The composites according to claim 7, wherein the content of NANO-HA in the composites is 10-50 wt %.