Flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel and preparation method thereof

A technology of hydroxyapatite and microcrystalline cellulose, which is applied in the fields of phosphorus compounds, chemical instruments and methods, colloid chemistry, etc., can solve problems such as no public reports on composite airgel research, and achieve excellent biocompatibility and Environmental friendliness, improved fire safety, low cost effects

Active Publication Date: 2018-07-03
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] So far, there have been no public reports on the preparation of comp...

Method used

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  • Flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel and preparation method thereof
  • Flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel and preparation method thereof
  • Flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 5.904g of calcium nitrate [Ca(NO 3 ) 2 4H 2 O] was dissolved in 25mL deionized water, and weighed 1.725g of ammonium dihydrogen phosphate (NH 4 h 2 PO 4 ) was dissolved in 25mL deionized water, and the above two solutions were mixed and stirred evenly, wherein the molar ratio of Ca / P was 5:3; the pH of the mixed solution was adjusted to 10 with 25% ammonia water, and reacted in a 40°C water bath for 1h ; transfer the above solution to the reaction kettle, and react at 180°C for 16h; after the reaction, cool to room temperature, open the kettle, centrifuge the solution, wash 3 times with deionized water, the centrifugal speed is 6000r / min, and the time is 8min. Finally, it was dried in an oven at 70° C. for 24 hours, and the obtained product was hydroxyapatite nanorods. Weigh 2.5g of hydroxyapatite nanorods and disperse them in 22.5mL of water, the content of hydroxyapatite is 10%, and ultrasonically stir for 2h to prepare a uniformly dispersed hydroxyapatite ...

Embodiment 2

[0030] Weigh 7g of sodium hydroxide and 12g of urea and dissolve them in 81mL of deionized water, place the solution in a freezer at -12°C for 20 minutes, weigh 6g of microcrystalline cellulose and slowly add it to the above solution, and stir for 0.5h until complete Dissolved, transferred to a three-necked bottle equipped with a mechanical stirring device and placed in a low-temperature water tank at 0°C, slowly added 4 mL of epichlorohydrin dropwise, and mechanically stirred for 1 hour to obtain a microcrystalline cellulose solution.

[0031] The above solution was placed in a constant temperature drying oven at 50°C for 12 hours to prepare microcrystalline cellulose hydrogel; the above hydrogel was rinsed with water to pH = 7, put into a freezer at -56°C for 12 hours, and then placed in a Dry in a vacuum freeze dryer for 120 hours, and the obtained product is microcrystalline cellulose airgel.

Embodiment 3

[0033]Weigh 25.4g of the microcrystalline cellulose solution prepared in Example 2 and 4.6g of the hydroxyapatite dispersion prepared in Example 1, mix the two and stir evenly, wherein the hydroxyapatite is mixed in microcrystalline cellulose / hydroxyphosphorus The content of the limestone composite airgel is 25%, and the microcrystalline cellulose / hydroxyapatite composite hydrogel is obtained by standing in a constant temperature drying oven at 50°C for 12 hours; the above hydrogel is rinsed with water until pH=7 , placed in a freezer at -56°C for 12 hours, and then dried in a vacuum freeze dryer for 96 hours. The resulting product is a flame-retardant microcrystalline cellulose / hydroxyapatite composite airgel.

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Abstract

The invention provides flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel and a preparation method thereof, relating to the fields of composite aerogel and a preparation method thereof. The preparation method comprises the steps of firstly synthesizing hydroxyapatite nanorods by virtue of a hydrothermal method, dispersing the hydroxyapatite nanorods into deionized water soas to prepare hydroxyapatite dispersion liquid, preparing a microcrystalline cellulose solution by taking a sodium hydroxide/urea water solution as a solvent and epoxy chloropropane as a cross-linking agent, finally, preparing flame-retardant microcrystalline cellulose/hydroxyapatite composite aerogel with a honeycomb structure by virtue of the cooperation of a solution blending method and a vacuum freeze drying method, wherein the hydroxyapatite nanorods with the diameters of 1nm-100nm and the lengths of 10nm-300nm are uniformly dispersed into a microcrystalline cellulose matrix. The prepared composite aerogel has obvious flame retardant effect and smoke release inhibition effect, the safety of aerogel in the fire is remarkably improved, and the adopted microcrystalline cellulose and hydroxyapatite have excellent biocompatibility and environmental friendliness.

Description

technical field [0001] The invention relates to the field of composite airgel and its preparation, in particular to a microcrystalline cellulose / hydroxyapatite composite airgel with excellent flame retardancy and smoke suppression performance obtained by using hydroxyapatite and its preparation method . Background technique [0002] Airgel is a nanoporous network structure composed of colloidal particles or polymer molecules aggregated with each other, and a highly dispersed solid nanomaterial filled with gaseous dispersion medium in the nanopores. The characteristics of airgel, such as low density, high specific surface area and high porosity, endow it with excellent heat insulation, heat preservation, sound resistance, adsorption and other properties, making it occupy an important position in the fields of mechanics, heat, optics, electromagnetics and electrochemistry. pivotal position. Airgel can be divided into inorganic aerogel, organic aerogel and inorganic / organic c...

Claims

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Application Information

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IPC IPC(8): C01B25/32B01J13/00
CPCB01J13/00C01B25/327
Inventor 鲁红典平鹏杨伟王宁宁杨本宏
Owner HEFEI UNIV
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