A method for preparing nanocellulose by multi-site oxidation method and its application

A nanocellulose and cellulose technology, applied in the field of cellulose, can solve the problems of difficulty in recycling, expensive enzymes, low reaction efficiency, etc., to reduce energy consumption and production costs, save mechanical defibrillation steps, and simplify the process. Easy to operate effect

Active Publication Date: 2018-09-14
NORTHEAST AGRICULTURAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Physical methods mainly include high-pressure homogeneous method, micro-jet method, disc grinding and ultrasonic method, etc. The main disadvantage of physical method is high energy consumption.
The chemical method uses inorganic strong acid and strong alkali to treat cellulose. Strong acid and strong alkali are corrosive to equipment and difficult to recycle. Waste liquid treatment is difficult and pollutes the environment.
Enzymes in biological methods are more expensive and the reaction conditions are harsh, and the reaction efficiency is low and the reaction time is long

Method used

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  • A method for preparing nanocellulose by multi-site oxidation method and its application
  • A method for preparing nanocellulose by multi-site oxidation method and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 500 ml of distilled water to a 1L beaker, wrap aluminum foil around it, add 2.5mmol TEMPO, 40mmol NaBr, 10mmol NaIO 4 Add to the beaker, cover the top with aluminum foil, and stir vigorously for 5 minutes with a magnetic stirrer. Remove the aluminum foil from the upper part of the beaker, and add 5 g of commercial microcrystalline cellulose into the beaker while continuing to stir with the magnetic stirrer. After stirring well, add 40 mmol NaClO slowly. The reaction was continuously stirred for 9 hours. During the reaction period, the pH value was adjusted with 2M NaOH every 1.5 hours to maintain the pH value of the reaction solution at about 10.5. After 9 hours of reaction, 5 mL of absolute ethanol was added to terminate the reaction, and the reaction time was 10 minutes. The reaction solution was centrifuged at 3000 rpm for 2 minutes, the supernatant was precipitated with absolute ethanol at a volume ratio of 1:1.2, and then centrifuged. The precipitate was wash...

Embodiment 2

[0033] Except that the reaction time is 4 hours, the rest of the operation method is the same as that in Example 1, and the nano cellulose with a rod-like shape can also be obtained by electron microscope observation.

Embodiment 3

[0035] Prepare nano cellulose with ordinary wood pulp as raw material. First, the general method is used to remove hemicellulose and lignin from wood pulp. Removal of lignin with glacial acetic acid and sodium chlorite, and removal of hemicellulose with potassium hydroxide to obtain purified cellulose. The following operation method is the same as that in Example 1, to obtain nanofibers with rod-shaped observation under electron microscope. Element, but there are more network structures (such as figure 2 ).

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Abstract

The invention relates to a method for preparing nano-crystalline cellulose by a multi-site oxidation method. The method comprises the following steps: adding cellulose raw materials into reaction liquid, continuously stirring and reacting for 4.5-18.0 hours under a specific pH (Potential of Hydrogen) value; terminating reaction by absolute ethyl alcohol; carrying out centrifugation, precipitant sedimentation, cleaning solution washing and filter membrane suction filtration on a reaction product to obtain the nano-crystalline cellulose, wherein the reaction liquid is the mixture of TEMPO (2,2,6,6-Tetramethylpiperidinooxy), periodate, sodium bromide and sodium hypochlorite, oxidizing substances are TEMPO, periodate and sodium hypochlorite; the periodate selectively oxidizes C2 and C3 site hydroxyl, TEMPO selectively oxidizes a C6 site hydroxyl, and therefore, the method is called a multi-site oxidation method. The multi-site oxidization process of the method is finished in one step, processing time is short, and a technology is simple; oxidization and fiber separation processes are simultaneously carried out, a mechanical fiber separation step is not required, energy consumption is low, and a separation and purification method is simple and is suitable for industrial scale production. The prepared nano-crystalline cellulose has a wide application prospect in fields including nanocomposite materials, functional clothes, 3D printing and photoelectricity and the like.

Description

Technical field [0001] The invention belongs to the technical field of cellulose, and particularly relates to a method for preparing nano cellulose by a multi-site oxidation method and its application. Background technique [0002] Nanocellulose is a cellulose material with a dimension of less than 100 nm in one dimension in three dimensions. Nano-cellulose has small size effect, surface interface effect and macroscopic quantum tunneling effect. It exhibits unique optical, electrical, magnetic and chemical properties. It is known as the "most promising material in the 21st century", which has attracted governments and scientific communities. It has a broad application prospect in the research of new materials and new technologies. [0003] Because adjacent cellulose microfibrils are chemically cross-linked or physically entangled, high-efficiency nano-fibrillated cellulose has always been a difficult point in the high-value utilization of cellulose. The preparation methods of nan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21H11/20C08B15/00
CPCC08B15/00D21H11/20
Inventor 孙孝政宋丽英裴熙祥
Owner NORTHEAST AGRICULTURAL UNIVERSITY
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