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Modified halloysite nanotube / biodegradable polyester composite material and preparation method thereof

A halloysite nanotube and biodegradable polyester technology, applied in the field of medical composite materials, can solve the problems of unsatisfactory mechanical properties and insufficient mechanical strength of biodegradable polyester, and achieve easy mass production and good biocompatibility. , the effect of the simple method

Inactive Publication Date: 2014-06-04
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem of insufficient mechanical strength of the existing biodegradable polyester, and overcome the inorganic particle / polymer nanocomposite caused by the uneven dispersion of inorganic particles and easy agglomeration in the existing inorganic particle / polymer nanocomposite materials Due to the unsatisfactory mechanical properties of materials, the primary purpose of the present invention is to provide a method for preparing a modified halloysite nanotube / biodegradable polyester composite material. A suitable organic group is covalently bonded, and the introduced organic group serves as a bridge between the inorganic particle and the polymer, which can make the modified halloysite nanotubes uniformly dispersed in the polymer matrix, which will effectively improve the performance of halloysite nanotubes. Interfacial bonding between the tube and the polymer, which ultimately increases the mechanical strength and modulus of the material

Method used

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  • Modified halloysite nanotube / biodegradable polyester composite material and preparation method thereof
  • Modified halloysite nanotube / biodegradable polyester composite material and preparation method thereof
  • Modified halloysite nanotube / biodegradable polyester composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation of modified halloysite nanotubes comprises the following steps:

[0038]In a three-necked flask, vacuum-dried halloysite nanotubes (30 g) were dispersed in tetrahydrofuran, and D,L-lactic acid (300 mL, 361 g) was slowly added through a dropping funnel under stirring conditions. After the addition was complete, React at 50°C for 6h, then distill off the solvent. Add 400mL of anhydrous toluene, azeotropic dehydration reaction at 110°C for 5h. After the reaction, the product was separated by high-speed centrifugation, and the supernatant was removed to obtain a solid product. The solid product was washed alternately and repeatedly ultrasonically with chloroform and absolute ethanol to remove lactic acid monomers adsorbed on the surface of the solid product. Finally, the solid product was collected by high-speed centrifugation and dried in vacuum to obtain halloysite nanotubes (l-HNTs) grafted with lactic acid on the surface.

[0039] Disperse the vacuum-d...

Embodiment 2

[0042] The preparation of modified halloysite nanotubes comprises the following steps:

[0043] In a three-necked flask, vacuum-dried halloysite nanotubes (50 g) were dispersed in tetrahydrofuran, and L-lactic acid (500 mL, 603 g) was slowly added through a dropping funnel under stirring conditions. The reaction was carried out at °C for 12 h, and then the solvent was distilled off. Add 400 mL of anhydrous toluene, and conduct azeotropic dehydration reaction at 110° C. for 10 h. After the reaction, the product was separated by high-speed centrifugation, and the supernatant was removed to obtain a solid product. The solid product was washed alternately and repeatedly ultrasonically with chloroform and absolute ethanol to remove lactic acid monomers adsorbed on the surface of the solid product. Finally, the solid product was collected by high-speed centrifugation and dried in vacuum to obtain halloysite nanotubes grafted with lactic acid on the surface.

[0044] Disperse the v...

Embodiment 3

[0047] The preparation of modified halloysite nanotube / poly (L-lactic acid) nanocomposite material comprises the following steps:

[0048] Mix HNTs, l-HNTs and p-HNTs (l-HNTs and p-HNTs are the products of Example 1) with poly(L-lactic acid) (PLLA) particles with a number average molecular weight of 300,000, and mix them uniformly at 180°C Plate-like HNTs / PLLA, l-HNTs / PLLA and p-HNTs / PLLA nanocomposites were obtained by injection molding with a precision injection machine, wherein the mass ratio of nanotubes in the composites was 2.5-40%. The bending performance of the nanocomposite obtained from the test is shown in the table below, and the cross-sectional morphology of the material is shown in image 3 .

[0049]

[0050] The data in the above table show that the flexural strength and flexural modulus of the l-HNTs / PLLA and p-HNTs / PLLA nanocomposite groups are significantly higher than those of the corresponding HNTs / PLLA nanocomposite group and single PLLA material. Th...

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Abstract

The invention discloses a modified halloysite nanotube / biodegradable polyester composite material and a preparation method and application thereof. The preparation method of the composite material comprises the following steps: synthesizing halloysite nanotube with lactic acid or polylactic acid grafted on the surface by a dehydration condensation reaction; and then preparing the halloysite nanotube with lactic acid or polylactic acid grafted on the surface and biodegradable polyester into a modified halloysite nanotube / biodegradable polyester composite material by a melt blending method, a solution blending method or an electrostatic spinning method. According to the invention, grafting modification is carried out on the halloysite nanotube surface, so as to effectively solve dispersion, stability and compatibility of two phases of the halloysite nanotube in a biodegradable polyester matrix, and endow the nano composite material with excellent mechanical properties.

Description

technical field [0001] The invention belongs to the field of medical composite materials, and in particular relates to a biodegradable polyester composite material reinforced by modified halloysite nanotubes, a preparation method and application thereof. Background technique [0002] Biodegradable polyesters such as polylactide (PLA), polyglycolide (PGA), poly(ε-caprolactone) (PCL) and their copolymers have good biocompatibility and mechanical strength and excellent Its processing performance is currently widely used in various fields of biomedicine, such as: fracture internal fixation materials, tissue engineering scaffold materials, drug release carrier materials, surgical sutures, etc.; however, as hard tissue repair materials such as fracture internal fixation materials, The mechanical strength of such biodegradable polyester materials is still not ideal. The mechanical properties of these materials can be effectively improved by adding inorganic particles, especially n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L67/04C08L69/00C08K9/04C08K7/00C08K3/34D04H1/435D04H1/728A61L31/06A61L27/18A61K47/34
Inventor 罗丙红文伟谢伟静章锦禧刘明贤周长忍
Owner JINAN UNIVERSITY
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