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Composite aerogel microsphere and preparation method thereof

A composite airgel and aerogel technology, applied in the field of nanocomposite materials and biomaterials, to achieve the effects of high production efficiency, improved mechanical strength, and increased surface active groups

Inactive Publication Date: 2018-09-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are no patent literature and non-patent literature reports on hydroxyapatite / graphene oxide composite airgel microspheres

Method used

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  • Composite aerogel microsphere and preparation method thereof
  • Composite aerogel microsphere and preparation method thereof
  • Composite aerogel microsphere and preparation method thereof

Examples

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Embodiment 1

[0036] (1) Preparation of hydroxyapatite: 3mol / L of Ca(NO 3 ) 2 4H 2 O aqueous solution and 3.5mol / L (NH 4 ) 2 HPO 4 The aqueous solution was uniformly mixed according to the volume ratio of 2:1, so that the Ca / P molar ratio was maintained at 1.67±0.5. Adjust the pH value of the solution to alkaline (pH>11) with ammonia water, stir evenly with magnetic force at 40°C, and wait for electrostatic spraying for later use.

[0037] (2) Place ethyl acetate in an open Dewar flask with good heat preservation, and add a large amount of liquid nitrogen while stirring until a slush-like liquid nitrogen / ethyl acetate cooling bath is formed. Put the beaker containing toluene and n-hexane into a liquid nitrogen / ethyl acetate cooling bath to cool it as a receiving liquid, and at the same time, put the prepared hydroxyapatite solution into the syringe on the electrostatic spray device, and adjust the height of the syringe nozzle After making it a suitable distance from the receiving liqu...

Embodiment 2

[0040] (1) Preparation of graphite oxide: natural graphite was prepared as graphite oxide by the improved Hummer method.

[0041] (2) Preparation of graphene oxide aqueous dispersion: at room temperature, mix the prepared 0.5g graphite oxide with 100ml deionized water, place in an ultrasonic cleaner, 400W ultrasonic dispersion for 1h and fully stir to obtain evenly dispersed dark brown 5mg / mL graphene oxide dispersion.

[0042] (3) Preparation of hydroxyapatite / graphene oxide dispersion: Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 Dissolved in distilled water to prepare solutions with a concentration of 3mol / L and 3.5mol / L. Add 5 mg / mL of graphene oxide dispersion to Ca 2+ solution, stir evenly, so that the mass ratio of hydroxyapatite and graphene oxide in the mixed solution is 1:0.02. Add a certain volume of PO 4 3- solution (3.5mol / L), so that the molar ratio of Ca / P was kept at 1.67. Adjust the pH value to alkaline (pH ≥ 11) with ammonia water, and form a uniform hyd...

Embodiment 3

[0046] (1) Preparation of graphite oxide: natural graphite was prepared as graphite oxide by the improved Hummer method.

[0047] (2) Preparation of graphene oxide dispersion: at room temperature, mix 0.5g of graphite oxide and 100ml of deionized water, place in an ultrasonic cleaner, 400W ultrasonic dispersion for 1h and then fully stir to obtain a uniformly dispersed dark brown 5mg / ml graphite oxide dispersion.

[0048] (3) Preparation of zinc-doped hydroxyapatite / graphene oxide dispersion: 3mol / L Ca(NO 3 ) 2 4H 2 O, 2.76mol / L Zn(NO 3)2 ·6H 2 O was uniformly mixed at a volume ratio of 17.5:1, and a certain volume of 5 mg / mL graphene oxide dispersion was added to Ca 2+ / Zn 2+ In the solution, stir evenly (100-1000 rpm), so that the mass ratio of hydroxyapatite to graphene oxide in the mixed solution is 1:0.02. In an appropriate ratio, add 3.5mol / L PO 4 3- solution so that the [Ca+Zn] / P molar ratio was kept at 1.67. Adjust the pH value to alkaline (pH ≥ 11) with ammo...

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Abstract

The invention discloses a composite aerogel microsphere and a preparation method thereof. The preparation method comprises the steps that firstly, prepared graphene oxide is subjected to ultrasonic stripping to obtain a graphene oxide solution, and a Ca2+ solution, a PO43- solution and a Zn2+ solution are added, wherein the molar ratio of Ca2+ to PO43- is 1.17-2.17, and the mass ratio of hydroxyapatite to the graphene oxide is 1:0.1-1:10; secondly, ammonia water is added and stirred to form composite dispersion liquid; finally, the composite aerogel microsphere is obtained through spraying, cooling bath receiving, sieving and freeze drying. The method is free of environmental pollution, low in raw material cost and high in production efficiency; the prepared hydroxyapatite / graphene oxide aerogel microsphere is regular in morphology, adjustable in size, low in mass, small in density, high in porosity and large in specific surface area, is of a porous network structure, has excellent biocompatibility and antibacterial property, can effectively promote cell proliferation and can directly serve as a biological application material.

Description

technical field [0001] The invention relates to a composite airgel microsphere and a preparation method thereof, belonging to the technical field of nanocomposite materials and biomaterials. Background technique [0002] Graphene is a new type of two-dimensional material formed by the regular arrangement of carbon atoms in a honeycomb manner. It has superior mechanical properties, electrical properties, optical properties, and thermal properties, so it has attracted extensive attention from people in various fields. Constructing two-dimensional graphene into a three-dimensional graphene macroscopic material is an important method and approach to enable graphene to be truly applied to industrial production under the condition that the excellent properties of graphene are not destroyed. Graphene oxide (GO) is a highly oxidized form of chemically modified graphene, which has a large number of oxygen-containing groups such as carboxylic acid, epoxide, and hydroxyl group in its ...

Claims

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Application Information

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IPC IPC(8): A61L27/12A61L27/08A61L27/50A61L27/56A61L27/54C01B32/198
CPCA61L27/08A61L27/12A61L27/50A61L27/54A61L27/56A61L2300/404A61L2300/412C01B32/198
Inventor 夏和生玛丽亚·格拉热亚·劳西蒋瑶珮路易·安部拉索王占华拉瓦叶纳·马里罗
Owner SICHUAN UNIV
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