Preparation method for nano-sliver/cellulose nanocrystalline composite particle

A nanocrystalline composite and cellulose technology, applied in the direction of nanotechnology, can solve the problems of weakening the reinforcement effect of biodegradable polymer matrix materials, destroying high-strength and high-mode characteristics, and not being able to become a reduction point, so as to shorten the preparation cycle and chemical Fewer drugs, improve the effect of combination

Inactive Publication Date: 2012-11-14
DONGHUA UNIV
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Problems solved by technology

However, the preparation process is not only multi-step, but periodate needs to open the glucoside ring of CNC, thereby destroying its rigid structure. The enhancement effect of biodegradable polymer matrix materials
Liu et al. put the CNC obtained from the acid hydrolysis of microcrystalline cellulose in the NaClO / NaBr / 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO) co-oxidation system to selectively oxidize it. The C6 primary hydroxyl group can reduce the silver salt to nano-silver without destroying the glycoside ring. This kind of composite particle can strengthen the water-soluble polyurethane material and endow the nano-material with good antibacterial properties, but this method is time-consuming and requires many steps. The raw materials of TEMPO are expensive and TEMPO can only oxidize the primary hydroxyl group of C6, the hydroxyl groups of C2 and C3 will not be oxidized and cannot become the reduction point, and the loading of nano-silver is low (Liu H, Song J, Shang S, Song Z, Wang D .Cellulose nanocrystal / silver nanoparticle composites as bifunctional nanofillers within waterborne polyurethane.ACS Appl.Mater.Interfaces 2012;5:2413–2419)

Method used

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  • Preparation method for nano-sliver/cellulose nanocrystalline composite particle
  • Preparation method for nano-sliver/cellulose nanocrystalline composite particle

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add microcrystalline cellulose to the formic acid / sulfuric acid solution, wherein the solid-to-liquid ratio of microcrystalline cellulose to the mixed acid solution is 1:30g / mL, and the volume ratio of formic acid (5mol / L) to sulfuric acid (8mol / L) in the mixed acid solution 8:1, the mixed solution was reacted at 85°C for 10h, and after the reaction was completed, the reaction product was washed with deionized water until it was neutral, and the formylated cellulose nanocrystal (CNC) could be obtained; the formylated cellulose nanocrystal Add crystal liquid to 0.01mol / L silver ammonia solution, the solid-to-liquid ratio of aldylated CNC to silver ammonia solution is 1:100g / mL, the mixed solution is reacted at 85°C for 15min, after natural cooling, dilute with deionized water The reaction product is centrifuged several times to remove inorganic ions, and then the dispersion is freeze-dried to obtain a nano-silver / CNC composite material. After the material is tested by a f...

Embodiment 2

[0027] Add the cellulose fiber to the formic acid / oxalic acid solution, wherein the solid-liquid ratio of the cellulose fiber to the mixed acid solution is 1:80g / mL, and the volume ratio of formic acid (3mol / L) to oxalic acid (5mol / L) in the mixed acid solution is 7 : 1, the mixed solution was reacted at 90°C for 18h, and after the reaction was completed, the reaction product was washed with deionized water until it was neutralized, and the formylated cellulose nanocrystal (CNC) could be obtained; the formylated cellulose nanocrystal liquid Add 0.5mol / L silver-ammonia solution, the solid-liquid ratio of aldehylated CNC to silver-ammonia solution is 1:50g / mL, and the mixed solution is reacted at 70°C for 45min. After natural cooling, dilute the reaction product with deionized water , several times of centrifugation to remove inorganic ions, and then vacuum-dry the dispersion to obtain nano-silver / CNC composite material. After the material is tested by field emission scanning ele...

Embodiment 3

[0029]Add cotton to the formic acid / nitric acid solution, wherein the solid-liquid ratio of cotton to the mixed acid solution is 1:60g / mL, and the volume ratio of formic acid (8mol / L) to nitric acid (3mol / L) in the mixed acid solution is 9:1, mix The solution was reacted at 75°C for 15 hours. After the reaction was completed, the reaction product was washed with deionized water until it was neutral, and aldehyde-based cellulose nanocrystals (CNC) could be obtained; add 0.09mol / In the silver-ammonia solution of L, the solid-to-liquid ratio of the aldylated CNC to the silver-ammonia solution is 1:300g / mL, and the mixed solution is reacted at 72°C for 30min. After natural cooling, the reaction product is diluted with deionized water and centrifuged several times. Remove the inorganic ions, and then freeze-dry the dispersion to obtain the nano-silver / CNC composite material. After the material is tested by the field emission scanning electron microscope, the obtained aldehyde-forme...

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Abstract

The invention relates to a preparation method for a nano-sliver/cellulose nanocrystalline composite particle. The preparation method comprises the following steps of: (1) adding a cellulose raw material into an acid-mixed solution and reacting at the temperature of 50-90DEG C for 1-20 hours; after the reaction is ended, washing a reaction product with deionized water to neutral and obtaining aldehyde cellulose nanocrystalline; and (2) adding the aldehyde cellulose nanocrystalline into a silver nitrate solution; reacting at the temperature of 60-105DEG C for 10-60 minutes; and after naturally cooling, diluting a reaction product with the deionized water, centrifuging and then carrying out free drying or vacuum drying to obtain a nano-silver/CNC (Cellulose Nanocrystalline) composite material. The preparation method disclosed by the invention is simple and convenient in process, easy in operation and environment friendly and can be used for shortening the preparation period; the prepared CNC/nano-silver has the advantages of small size, easy adjustment, large specific area, firmness in combination of the CNC and the nano-silver, durable antibacterial effect, antibacterial and enhancing functions and broad application prospect.

Description

technical field [0001] The invention belongs to the field of preparation of functional nanoparticles, in particular to a method for preparing nano silver / cellulose nano crystal composite particles. Background technique [0002] Cellulose is an inexhaustible and inexhaustible renewable natural polymer synthesized mainly by plants through photosynthesis in nature. Cellulose microcrystals / nanocrystals extracted from natural cellulose have many excellent properties, such as high strength and high modulus (Young's modulus and tensile strength can reach 150GPa and 250MPa, respectively), good biocompatibility, Biodegradable, rich in highly reactive hydroxyl groups on the surface, high crystallinity and good shape retention, it has been widely used in food, medicine, cosmetics and paint stabilizers (such as CN101481424A; CN1448427A; CN1340651A), plastics and Rubber filler (such as CN1369508A; CN1340651A) and synthetic leather production (such as CN101070352A; CN1220271A). In parti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L1/08C08K3/08C08B15/00B22F9/24B82Y40/00
Inventor 秦宗益余厚咏刘彦男吴谦肖婉瑶李亚茹陈龙
Owner DONGHUA UNIV
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