Cellulose nanocrystals from renewable biomass

一种纳米晶体、纤维素的技术，应用在来自可再生生物质的纤维素纳米晶体领域，能够解决高初始投资、高运行费用、昂贵等问题，达到高产率、提高均匀性的效果

Inactive Publication Date: 2013-02-27
NAT RES COUNCIL OF CANADA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this approach is expensive, requiring a rather high initial investment and having high operating costs due to the corrosivity of these acids and their by-products, safety concerns and hazardous waste handling / disposal requirements

Method used

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  • Cellulose nanocrystals from renewable biomass
  • Cellulose nanocrystals from renewable biomass
  • Cellulose nanocrystals from renewable biomass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Preparation of Cellulose Nanocrystals (CNCs) by Persulfate

[0032] The method described in this example is an environmentally friendly one-step process for the preparation of CNCs from different cellulose products. Ammonium persulfate has very high solubility in cold water (85g / 100ml), while sodium persulfate (55.6g / 100ml) and potassium persulfate (5.3g / 100ml) have lower solubility (Weast, 1983). CNCs were prepared by simply heating the cellulosic material in 1M persulfate at 60°C with vigorous stirring for 16 hours, described in more detail below using ammonium persulfate as an example. Lignocellulosic fibers such as flax and hemp are cut into short pieces (about 2-3 mm) prior to persulfate treatment. Long reaction times and persulfate concentrations above 1 M lead to excessive hydrolysis, thereby reducing the yield of CNCs.

[0033] Therefore, in one example, starting biomass material (0.1 g) was added to 10 ml of 1M ammonium persulfate solution (approxi...

Embodiment 2

[0034] Example 2: Atomic Force Microscopy (AFM) and Transmission Electron Microscopy (TEM)

[0035] CNCs prepared using ammonium persulfate were sonicated, and atomic force microscopy (AFM) micrographs of the CNCs thus obtained were obtained using a Nanoscope TM IV (Digital Instruments, Veeco, Santa Barbara, Canada) was obtained by operating in tapping mode with a silicon tip. Particle Analysis of AFM Micrographs Using Scion TM images (http: / / www.scioncorp.com / pages / scion_image_windows.htm).

[0036] TEM micrographs were obtained by a Hitachi transmission electron microscope (TEM) at 60 kV (Model H-7500, Tokyo, Japan). TEMs were obtained as follows. A small amount of CNCs was suspended in methanol and the material was dispersed by sonication. 20 [mu]L droplets of the well-dispersed suspension were then dried on polyvinyl formal and vinyl chloride polyvinyl alcohol terpolymer (Formvar)-carbon coated grids and analyzed. Low-voltage transmission electron microscopy (LVTEM) m...

Embodiment 3

[0046] Example 3: Scanning Electron Microscope (SEM)

[0047] SEM analysis was performed by a Hitachi S2600N scanning electron microscope at 2.8 kV. SEM shows the morphological changes of the ammonium persulfate-treated fiber surface, indicating the destruction of the amorphous regions. In contrast, when the fibers were heated without ammonium persulfate, they remained intact. Ammonium persulfate enables the in situ preparation of clean CNCs by dissolving lignin, hemicellulose, pectin, and other plant components. When a solution containing persulfate is heated, free radicals (S 2 o 8 2- + heating → 2SO 4 ·- ) (Hsu et al., 2002). Therefore, persulfates are often used as initiators for emulsion polymerization in the preparation of polymers and synthetic rubbers. Furthermore, under the acidic conditions (pH 1.0) used in this study, hydrogen peroxide (S 2 o 8 2- +2H 2 O→HSO 4 - +H 2 o 2 ) (Edgar and Gray, 2003; Stiernstedt et al., 2006). Collectively, the free rad...

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Abstract

A process for producing cellulose nanocrystals (CNCs) involves providing a cellulosic material, contacting the cellulosic material with an inorganic persulfate at an elevated temperature to produce CNCs, and recovering the CNCs. The process permits one-step production of CNCs from vegetative biomasses such as flax and hemp. Cellulose nanocrystals produced by the process with carboxylic groups are more uniform and have higher aspect ratios than CNCs produced by prior art processes.

Description

[0001] Cross References to Related Applications [0002] This application claims the benefit of United States Provisional Patent Application Serial No. USSN 61 / 282,094, filed December 15, 2009, the entire contents of which are incorporated herein by reference. technical field [0003] The invention relates to a method for preparing cellulose nanocrystals from renewable biomass, and cellulose nanocrystals with carboxyl groups prepared by the method. Background technique [0004] According to French scientist Anselme Payen in 1838, cellulose has the molecular formula (C 6 h 10 o 5 ) n . It is the most abundant organic polymer, with about 1.5×10 12 used in tons. It has been used as a renewable, biodegradable and environmentally friendly chemical raw material for 150 years. Cellulose is semicrystalline, having crystalline and amorphous regions. It is densely packed with strong intermolecular and intramolecular hydrogen bonds, giving excellent mechanical properties. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/08C08B15/00C08H8/00C08L1/02
CPCC08B15/08C08B15/04Y10T428/2982
Inventor 梁子桓J·H·T·隆S·拉波维克E·拉姆刘亚力K·B·梅尔K·马哈穆德D·罗
Owner NAT RES COUNCIL OF CANADA
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