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Redispersable nanoparticle powder material preparation method

A technology of nanoparticles and powder materials, which is applied in the field of preparation of nano-particle powder materials, can solve the problems that it is difficult to avoid the re-aggregation of nanoparticles and the difficulty of re-dispersion of nano-particle materials, and achieve the effect of easy dispersion and convenient use.

Active Publication Date: 2013-07-24
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even with freeze-drying techniques, it is difficult to avoid the re-agglomeration of nanoparticles during the drying process, thus making the redispersion of nanoparticle materials a problem

Method used

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  • Redispersable nanoparticle powder material preparation method
  • Redispersable nanoparticle powder material preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1, preparation redispersible nano-cellulose whisker

[0028] Weigh the dry microcrystalline cellulose (polymerization degree 220) that has been vacuum-dried at 80°C for 12 hours and disperse it in secondary water, add concentrated sulfuric acid dropwise under ice bath to make the concentration of microcrystalline cellulose 10.2g / 100mL, sulfuric acid The mass concentration was 63.5%, and then heated to 44° C. within 5 minutes, mechanically stirred for 2 hours, and then centrifuged to remove the surface suspension (centrifugation until the upper layer was turbid). Ultrasonic dispersion of the resulting white slurry is followed by dialysis until the pH value remains constant, (at this time the concentration is greater than 1%) to obtain an aqueous solution of nanocellulose whiskers, and an appropriate amount of hydrochloric acid with a mass concentration of 36.5% is added to form a nanocellulose whisker / water solution. gel. The water in the gel was replaced wit...

Embodiment 2

[0029] Embodiment 2, preparation redispersible cellulose nanofiber

[0030] 1g of cellulose fibers was added to TEMPO (2,2,6,6-tetramethylpiperidine oxide) (0.016g), NaBr (0.1g) in 100mL aqueous solution, and then added dropwise with pH value of 12, NaClO The content is 12% aqueous solution, so that the final concentration of NaClO is 4 mmol. Then stir at room temperature, add dropwise 0.5M NaOH to adjust the pH value to be stable at about 10, until the dropwise addition of NaOH is no longer required. Then the obtained oxidized cellulose is treated with ultrasonic and homogenizer to obtain oxidized nanofibrils, and the obtained oxidized nanofibrils (containing -COONa) are washed to neutral with deionized water, and then the mass concentration of cellulose obtained after oxidation is Adjust to 0.1%, add dropwise 1M HCl under stirring condition, adjust the pH to 1, at this time a transparent cellulose nanofibril gel is formed. The gel is replaced with ethanol to obtain alcohol...

Embodiment 3

[0031] Embodiment 3, preparation redispersible lithium magnesium silicate particle

[0032] 2.5g dried lithium magnesium silicate powder (commodity ) was dispersed in 97.5mL of secondary water, mechanically stirred at room temperature for 4h to obtain a transparent nanoscale dispersion of lithium magnesium silicate; the resulting aqueous dispersion was allowed to stand overnight, during which the suspension gelled to obtain Lithium magnesium silicate hydrogel. The water in the hydrogel is replaced by ethanol until the water is completely replaced by ethanol, and then supercritical carbon dioxide is dried to obtain a solid lithium magnesium silicate nanoparticle powder material. The powder material obtained by drying is light blue. The lithium magnesium silicate nanoparticle powder material can be well redispersed in water and dimethyl sulfoxide, N,N-dimethylacetamide, N,N-dimethylformamide, pyridine and N-formaldehyde In polar organic solvents such as pyrrolidone.

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Abstract

The invention discloses a redispersable nanoparticle powder material preparation method. The method comprises the following steps: 1, dispersing polar nanoparticles in water through mechanical stirring or ultrasonic dispersion; 2, gelating a uniformly-dispersed nanoparticle / water suspension to obtain a nanoparticle hydrogel material; 3, carrying out alcohol solvent displacement of the nanoparticle hydrogel material to obtain a nanoparticle alcogel material; and 4, carrying out supercritical carbon dioxide drying of the nanoparticle alcogel material to obtain a solid nanoparticle powder material. The obtained solid nanoparticle powder material can be easily redispersed in water and a plurality of polar solvents. The method does not change the structure or properties of the nanoparticles, and the prepared redispersable nanoparticle powder material is easy to preserve and transport and is convenient to use.

Description

technical field [0001] The invention relates to a preparation method of a redispersible nano particle powder material. Background technique [0002] Nanomaterials refer to a class of materials whose structural units have at least one dimension ranging from 1 nanometer to 100 nanometers. Due to its size effect and its special effect of large specific surface area, the properties exhibited are often different from those of the substance in the macroscopic state, such as melting point, gas barrier, magnetism, optics, thermal conductivity, electrical conductivity, etc. Wait. Combining nanoparticles into polymers can produce polymer nanocomposites with special properties. However, due to their small size, nanoparticles have a high specific surface area, and the surface atoms are in a highly activated state, which makes the surface energy high and the particles are easy to agglomerate. Usually filled with nanoparticles without surface treatment, not only will not play a special...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/00C01B33/32C01B33/40C01B31/04B82Y40/00B82Y30/00C01B32/158C01B32/159C01B32/184C01B32/23
Inventor 张军王德修
Owner INST OF CHEM CHINESE ACAD OF SCI
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