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Method for preparing fibrilia carboxylation cellulose nanowhiskers

A technology of carboxylated cellulose and nanocrystals, applied in the direction of nanotechnology, can solve the problems of high crystallinity of hemp fibers, difficult cellulose nanocrystals, etc., and achieve the effects of good repeatability, simple preparation process and low energy consumption

Inactive Publication Date: 2012-09-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing hemp fiber carboxylated cellulose nanocrystals, to solve the technical problem that hemp fiber is difficult to prepare structurally uniform cellulose nanocrystals with high efficiency and high yield due to the high crystallinity

Method used

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  • Method for preparing fibrilia carboxylation cellulose nanowhiskers
  • Method for preparing fibrilia carboxylation cellulose nanowhiskers
  • Method for preparing fibrilia carboxylation cellulose nanowhiskers

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Under the temperature condition of 20 ℃ of water baths, 1.0g60 purpose jute fiber powder is soaked in the stirred kettle that fills 50g mass fraction and is 15% sodium hydroxide solution, stirs 120min with the stirring speed of 300rpm, then pumps out with vacuum pump Filter, wash the jute fiber powder of gained to neutrality, dry in vacuum oven, vacuum tightness is 0.1MPa, and drying temperature is 60 ℃, and drying time is 12h, obtains the jute fiber powder of alkali treatment;

[0033] (2) under the temperature condition of 70 ℃ of water baths, the jute fiber powder of alkali treatment that the first step obtains is joined in the stirred tank that fills dimethyl sulfoxide (DMSO), the jute fiber powder of alkali treatment and dimethyl The solid-to-liquid mass ratio of sulfoxide was 1:50, stirred for 4h at a stirring speed of 500rpm, filtered, and the residual dimethyl sulfoxide was eluted with distilled water, and the jute fiber powder was dried in a vacuum oven with...

Embodiment 2

[0038] (1) Under the temperature condition of 80 ℃ of water baths, 20g60 purpose flax fiber powders are soaked in the mass fraction that fills 200g and be 20% sodium hydroxide solution stirring tank, stir 100min with the stirring speed of 300rpm, then use vacuum pump suction filtration, The flax fiber powder obtained was washed to neutrality, and dried in a vacuum oven with a vacuum degree of 0.1 MPa, a drying temperature of 80° C., and a drying time of 6 hours to obtain alkali-treated flax fiber powder;

[0039] (2) Under the temperature condition of 70 ℃ of water baths, the flax fiber powder of alkali treatment that the first step obtains is joined in the stirred tank that fills the tetrabutylammonium bromide solution of 10% by mass fraction, the flax fiber powder of alkali treatment The solid-liquid mass ratio of powder and tetrabutylammonium bromide solution is 1: 20, stirs 6h with the stirring speed of 100rpm, suction filtration, with distilled water eluting residual tetra...

Embodiment 3

[0044] (1) under 60 ℃ of water-bath temperature conditions, 1g60 purpose jute fiber powder is soaked in the mass fraction that fills 40g and is in the stirred tank of 16% sodium hydroxide solution, stirs 300min with the stirring speed of 200rpm, then uses vacuum pump suction filtration, The jute fiber powder of gained is washed to neutrality, is dried in vacuum oven, and vacuum degree is 0.1MPa, and drying temperature is 70 ℃, and drying time is 12h, obtains the jute fiber powder of alkali treatment;

[0045] (2) under 70 ℃ of water-bath temperature conditions, the jute fiber powder of the alkali treatment that the first step obtains joins in the stirred tank that fills the massfraction of 30% methyl trioctyl ammonium chloride solution, the alkali treatment The solid-liquid mass ratio of jute fiber powder and methyl trioctyl ammonium chloride solution is 1: 20, stirs 4h with the stirring speed of 300rpm, suction filtration, residual methyl trioctyl ammonium chloride is washed w...

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Abstract

The invention provides a method for preparing fibrilia carboxylation cellulose nanowhiskers, which is characterized by comprising the following steps: soaking fibrilia powder in sodium hydroxide for processing, then processing the fibrilia powder by a former treating agent and taking out the fibrilia powder to be dried in a vacuum oven to obtain preprocessed fibrilia powder; and placing the preprocessed fibrilia powder in a TEMPO oxidation system for catalytic oxidation to obtain a stable cellulose nanowhiskers suspending liquid after mechanical processing and freeze drying the suspending liquid to obtain the fibrilia carboxylation cellulose nanowhiskers having grain diameters of 3-10 nm. According to the invention, fibrilia carboxylation and nano fibrillation are realized and surfaces of prepared nanocrystalline celluloses have carboxyl functional groups, thus the surfaces generate negative charges, electrostatic repulsion among the negative charges can avoid the reunion of nanoparticles, so that the nanocrystalline celluloses can be well dispersed in water and the obtained nanocrystalline celluloses have excellent uniformity of grain sizes.

Description

technical field [0001] The invention relates to a method for preparing hemp fiber carboxylated cellulose nano crystals, belonging to the technical field of nano functional materials. Background technique [0002] Cellulose nanocrystals (Cellulose Nanohiskers) are nanomaterials separated from natural cellulose fibers with a diameter between 1 and 100 nm and a granular, rod (needle) or filamentary structure. Due to the advantages of renewability, high strength, high elastic modulus, high specific surface area, low cost, biodegradability, and nanoscale fine scale, it has attracted extensive attention. Patent CN1334273A discloses a preparation method of nano-microcrystalline cellulose by using a strong acid method. Due to the use of a large amount of strong acid, the environmental pollution is serious, the equipment requirements are high, and the output is relatively low. Patent CN101851801A discloses a method for preparing nanocellulose fibers combined with ultrasound and high...

Claims

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Application Information

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IPC IPC(8): C08B15/04C08B15/08B82Y40/00
Inventor 丁彬曹新旺任韬俞建勇
Owner DONGHUA UNIV
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