Cellulose nanofibers and preparation method thereof

A nanofiber and cellulose technology, applied in the field of cellulose nanofiber and its preparation, can solve the problems of long cycle and strict environmental conditions, high requirements for machinery and equipment, high energy consumption, etc., and achieve high modifiability, excellent Mechanical properties, the effect of reducing energy consumption

Active Publication Date: 2022-07-05
WUHAN UNIV
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  • Application Information

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Problems solved by technology

For example, at the earliest, people used a high-pressure homogenizer to vibrate fibers in water to obtain cellulose nanofibers, and later derived ultrasonic methods, ball milling methods, etc. can produce cellulose nanofibers, but these methods need to consume a lot of energy, and The requirements for machinery and equipment are high; in addition, the method of using chemical pretreatment to destroy some hydrogen bonds in cellulose and to charge cellulose can reduce the energy consumption of subsequent mechanical treatment to a certain extent, but the toxicity of chemical reagents cannot be avoided , Decreased structural stability of cellulose and other issues; biological enzyme method can obtain cellulose nanofibers with complete structure relatively mildly, but the yield is low, requiring a long period and strict environmental conditions

Method used

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  • Cellulose nanofibers and preparation method thereof
  • Cellulose nanofibers and preparation method thereof
  • Cellulose nanofibers and preparation method thereof

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preparation example Construction

[0035] The invention provides a cellulose nanofiber and a preparation method thereof.

[0036] Preparation method of cellulose nanofibers

[0037] The preparation method of cellulose nanofibers comprises the following steps:

[0038] Step 1): disperse the cellulose in the first organic solvent and configure it into a cellulose dispersion;

[0039] Step 2): adding lithium hydroxide to the cellulose dispersion obtained in step 1) to fully swell the cellulose;

[0040] Step 3): react the fully swollen cellulose obtained in step 2) with an acid anhydride, wash the reaction solution, and obtain a cellulose reaction product;

[0041] Step 4): Disperse the cellulose reaction product obtained in step 3) in an alkaline aqueous solution, centrifuge, and dialyze the supernatant to obtain a suspension containing cellulose nanofibers.

[0042] In one or more embodiments of the present invention, in the step 1), the first organic solvent is dimethyl sulfoxide.

[0043] In one or more em...

Embodiment 1

[0056] Under anhydrous conditions, the ascidian cellulose raw material was dispersed in dimethyl sulfoxide to form a 0.5wt% dispersion liquid, lithium hydroxide was added to fully swell the cellulose, and the mass ratio of the added lithium hydroxide to cellulose was 1 : 5. Add succinic anhydride in a molar ratio of 1:1 (acid anhydride: anhydroglucose unit), stir magnetically, and react for 1 h. The reaction temperature is controlled to 15 °C. After the reaction is complete, dimethyl sulfoxide and ethanol are used for centrifugal washing in turn to obtain cellulose. The reaction product, the cellulose reaction product was dispersed in an aqueous lithium hydroxide solution with pH=8, and dialyzed for three days to obtain a suspension containing cellulose nanofibers. The yield of the obtained cellulose nanofibers was about 10%, and the average diameter was about 10%. It is 12 nm, the height is between 4 and 8 nm, the length is between 10 and 15 μm, and the aspect ratio is betwee...

Embodiment 2

[0058] Under anhydrous conditions, the ascidian cellulose raw material was dispersed in dimethyl sulfoxide to form a 1wt% dispersion liquid, lithium hydroxide was added to fully swell the cellulose, and the mass ratio of the added lithium hydroxide to the cellulose was 1: 10. Add phthalic anhydride in a molar ratio of 3:1 (acid anhydride: anhydroglucose unit), stir magnetically, react for 12 hours, and control the reaction temperature to 25 °C. The reaction product, the cellulose reaction product was dispersed in a lithium hydroxide aqueous solution with pH=11, and dialyzed for three days to obtain a suspension containing cellulose nanofibers. The yield of the obtained cellulose nanofibers was about 45%, and the average diameter was about It is 12 nm, the height is between 4-8 nm, the length is between 10 and 15 μm, and the aspect ratio is between 800 and 1250.

[0059] figure 1 is the atomic force microscope image of the ascidian cellulose nanofibers obtained by the prepara...

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Abstract

The present invention provides a method for preparing cellulose nanofibers, comprising the following steps: Step 1): dispersing cellulose in a first organic solvent to prepare a cellulose dispersion; Step 2): adding the fibers obtained in step 1) to Lithium hydroxide is added to the cellulose dispersion to fully swell the cellulose; step 3): react the fully swollen cellulose obtained in step 2) with an acid anhydride, wash the reaction solution, and obtain a cellulose reaction product; step 4): the step 3) The obtained cellulose reaction product is dispersed in an alkaline aqueous solution, centrifuged, and the supernatant is dialyzed to obtain a suspension containing cellulose nanofibers. The preparation method provided by the invention has wide and readily available raw materials, only needs simple and mild magnetic stirring, the whole process can be carried out at room temperature, the reaction conditions are mild, and the cost is low. The prepared cellulose nanofibers have an aspect ratio of >800, higher modifiability and excellent mechanical properties.

Description

technical field [0001] The patent of the present invention relates to the fields of chemical engineering and polymer functional materials, especially cellulose nanofibers and their preparation methods. Background technique [0002] Cellulose is a class of natural linear polymers with abundant reserves and the most widely distributed in the world. It is environmentally friendly, green and degradable. In recent years, it has been found that cellulose one-dimensional or two-dimensional materials can be obtained after chemical or mechanical treatment under suitable conditions. This discovery is expected to further expand the application range of cellulose. Among them, microfibrillated cellulose nanofibers have been proposed to have ultra-high aspect ratios and excellent mechanical properties, so they are widely used as reinforcements for nanofillers and polymers. At the same time, the reduction of particle size enables cellulose nanofibers to have larger specific surface area a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F2/28B82Y40/00
CPCD01F2/28B82Y40/00
Inventor 常春雨周盟
Owner WUHAN UNIV
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