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Preparation method of noble metal nanoparticle-cellulose hybrid membrane

A cellulose and hybrid membrane technology, which is applied in the field of preparation of nano-precious metal particles-regenerated cellulose hybrid membrane, can solve the problems of uneven shape, difficulty in realizing industrialized production, and difficulty in controlling dispersion, and achieves a simple preparation method. Effect

Inactive Publication Date: 2012-02-15
NAT UNIV OF DEFENSE TECH
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Problems solved by technology

The preparation method of this kind of nano-noble metal particles-cellulose hybrid material relies too much on the structure and properties of the cellulose porous material, and the prepared nano-noble metal particles have uneven particle size and shape, and it is difficult to control their dispersion.
In 2008, Shingo Yokota et al. tried to use thiosemicarbazone-grafted low-polymerization cellulose dissolved in N-methylmorpholine oxide (NMMO) for direct hybridization with nano-gold (Au) particles. However, it failed due to the agglomeration of gold nanoparticles and the inability to redisperse (Angew.Chem., 2008, 120: 10014~10017)
The present inventor once used NMMO solvent method to prepare cellulose solution, and successfully solved the phenomenon that nano-gold particles were agglomerated in NMMO solution by using cheap dimethyl sulfoxide (DMSO) as a co-solvent, and proposed a method for preparing An effective method for nano-gold particle-cellulose hybrid membrane (Chem.Mater., 2010, 22(8): 2675-2680), which uses gold sol to directly regenerate cellulose dissolved in NMMO, and the utilization of nano-gold particles The ratio and its dispersion in the cellulose film are greatly affected by the content of NMMO, suitable for laboratory research, but difficult to achieve industrial production

Method used

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  • Preparation method of noble metal nanoparticle-cellulose hybrid membrane

Examples

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Embodiment 1

[0031]At 90°C under the protection of nitrogen, add 2g of α-cellulose to 98g of NMMO H2O, and continue stirring for 2 hours to obtain a cellulose solution; The smooth silicate glass sheet is used as the substrate, and the cellulose solution dissolved at 70°C is used to spin the film on the surface of the spin coating machine to prepare the cellulose solution film, and the rotation speed is set at 1krpm; the cellulose is soaked in deionized water After the solution was smeared for 2 hours, the regenerated cellulose membrane was rinsed and stored in deionized water; 1.5 g of chloroauric acid (HAuCl 4 ) was dissolved in 4.5L deionized water, and the chloroauric acid solution was heated to boiling under magnetic stirring, and 4.5g sodium citrate (Na 3 C 6 h 5 o 7 ) was dissolved in 0.5L deionized water, and after dissolving, the sodium citrate solution was quickly added to the boiling chloroauric acid solution, and the heating was continued for 25 minutes, then the heating was ...

Embodiment 2

[0033] At 90°C under nitrogen protection, 8 g of cotton pulp cellulose and 0.05 g of propyl gallate were added to 92 g of NMMO·H 2 In O, after 24 hours of continuous stirring, a cellulose solution was obtained; under the conditions of a temperature of 30° C. and a relative humidity RH=30%, the cellulose solution dissolved at 90° C. was extruded and blown into a film by a film blowing machine, and passed The cellulose is regenerated by the sink, and the regenerated cellulose film is fully rinsed with water vapor; the 56g potassium chloroplatinate (K 2 PtCl 6 ) was dissolved in 57.6L deionized water, and the potassium chloroplatinate solution was heated to boiling under magnetic stirring; 98.4g citric acid (H 3 C 6 h 5 o 7 ) was dissolved in 6.4L deionized water, and after being fully dissolved, the sodium citrate solution was quickly added to the boiling potassium chloroplatinate solution, and the heating was continued for 25 minutes, then the heating was stopped, and the p...

Embodiment 3

[0035] At 90°C under nitrogen protection, 8 g of straw pulp cellulose was added to 32 g of NMMO·H 2 O, after continuous stirring for 12 hours, a cellulose solution was obtained, 80 g of DMSO was added thereto, and at 70° C., continued stirring for 12 hours to obtain a uniformly mixed film-forming liquid; Under certain conditions, after the film-forming solution at 75°C was left to stand for 20 minutes, the mica sheet was used as the base, and the clean substrate was dipped-pulled to form a film at a pulling speed of 15cm / min; use excess deionized water to soak the smear 2 hours, then fully rinse the regenerated cellulose membrane; at room temperature, 1.2g silver nitrate (AgNO 3 ) was dissolved in 14.4L deionized water, fully dissolved under medium-speed stirring; 3.9g potassium citrate (K 3 C 6 h 5 o 7 ) was dissolved in 1.6L deionized water, and after being fully dissolved, the potassium citrate solution was quickly added to the silver nitrate solution; after stirring co...

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Abstract

The invention relates to a preparation method of a nanometer metal-cellulose hybrid membrane, especially to a preparation method of a noble metal nanoparticle-cellulose hybrid membrane. By steps of preparing a cellulose solution, preparing a membrane by the cellulose solution, preparing noble metal nanosol, preparing the nanometer metal-cellulose hybrid membrane and the like, the noble metal nanosol is used as a noble metal source, and the self-assembly of the noble metal nanosol on the surface of the industrial regenerated cellulose membrane is realized by the irreversible diffusion process so as to prepare the high surface enriched noble metal nanoparticle-cellulose hybrid membrane. The prepared noble metal nanoparticle-cellulose hybrid membrane has excellent assembly and fixing performance for guest substances such as proteins and enzyme, and can be widely applied in the construction of nanometer dielectric conductors, bioactive molecular membranes, biochemical sensors and the like.

Description

technical field [0001] The invention relates to a preparation method of a nanometer metal-cellulose hybrid film, in particular to a preparation method of a nanometer precious metal particle-regenerated cellulose hybrid film. Background technique [0002] Nano-metal-polymer hybrid materials not only have the excellent mechanical properties of polymers, but also retain the functional properties of nano-metals. Under the synergistic effect of multiple components, they have unique force, heat, sound, light, electricity and magnetic and other performance. As the most abundant renewable resource in nature, cellulose is the main material composition of plants and has high biocompatibility and degradability. In recent years, it has become a research hotspot in the field of nanomaterials to hybridize nanometals with the functions of conductivity, wave absorption, catalysis, and biochemical detection into cellulose membranes. [0003] In 2004, Junhui He et al. published an article o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J7/00C08J7/12C08J3/09C08L1/02
Inventor 刘志明吴文健胡碧茹满亚辉
Owner NAT UNIV OF DEFENSE TECH
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