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Method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis in combination with ultrasonic assistance

A nanocellulose, ultrasonic-assisted technology is applied in the field of green preparation of nanocellulose to achieve the effects of reducing process and drug consumption, stable dispersion and high yield

Pending Publication Date: 2019-05-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no report on the one-step preparation of carboxylated nanocellulose with high yield by citric acid hydrolysis combined with ultrasonic assistance.

Method used

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  • Method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis in combination with ultrasonic assistance
  • Method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis in combination with ultrasonic assistance
  • Method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis in combination with ultrasonic assistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Preparation of carboxylated nanocellulose by citric acid hydrolysis combined with ultrasound-assisted one-step method

[0040] (1) At a temperature of 100°C, 5g of dry bleached bagasse pulp board was pulverized and added to an aqueous citric acid solution (80g citric acid, 20ml deionized water) with a concentration of 80wt% for 4 hours to obtain a hydrolysis suspension.

[0041] (2) Vacuum filtration of the hydrolyzed suspension through a G4 sand core funnel to obtain solid fibers and filtrate. The fibers were repeatedly added with deionized water and centrifuged at 4000 r / min to wash until neutral, and the filtrate was subjected to rotary evaporation at 70 °C and 60 r / min to obtain a white citric acid crystalline solid.

[0042] (3) The washed fibers were sonicated at 900W for 20min by an ultrasonic cell crusher (there was a 5s interval after each 5s of sonication). After the sonication, 200ml of deionized water was added and sonicated for 20min.

[0043](4...

Embodiment 2

[0045] Example 2: Preparation of carboxylated nanocellulose by citric acid hydrolysis combined with ultrasound-assisted one-step method

[0046] (1) At a temperature of 100°C, add 5g of dry bleached bagasse pulp board to a citric acid aqueous solution (70g citric acid, 30ml water) with a concentration of 70wt% for 4h to obtain a hydrolysis suspension.

[0047] (2) Vacuum filtration of the hydrolyzed suspension through a G4 sand core funnel to obtain solid fibers and filtrate. The fibers were repeatedly added with deionized water and centrifuged at 4000 r / min to wash until neutral, and the filtrate was subjected to rotary evaporation at 70 °C and 60 r / min to obtain a white citric acid crystalline solid.

[0048] (3) The washed fibers were sonicated at 900W for 20min by an ultrasonic cell crusher (there was a 5s interval after each 5s of sonication). After the sonication, 200ml of deionized water was added and sonicated for 20min.

[0049] (4) After centrifuging the cellulose s...

Embodiment 3

[0051] Example 3: Hydrolysis of citric acid combined with ultrasonic-assisted one-step preparation of carboxylated nanocellulose

[0052] (1) At a temperature of 100°C, 5g of dry bleached wood pulp board was pulverized and added to an aqueous solution of citric acid (80g citric acid, 20ml water) with a concentration of 80wt% for 4h to obtain a hydrolysis suspension.

[0053] (2) Vacuum filtration of the hydrolyzed suspension through a G4 sand core funnel to obtain solid fibers and filtrate. The fibers were repeatedly added with deionized water and centrifuged at 4000 r / min to wash until neutral, and the filtrate was subjected to rotary evaporation at 70 °C and 60 r / min to obtain a white citric acid crystalline solid.

[0054] (3) The washed fibers were sonicated at 900W for 20min by an ultrasonic cell crusher (there was a 5s interval after each 5s of sonication). After the sonication, 200ml of deionized water was added and sonicated for 20min.

[0055] (4) After centrifuging ...

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Abstract

The invention discloses a method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis in combination with ultrasonic assistance. The method comprises the steps: selecting a bleached fiber pulp board as a substrate; then, adding the bleached fiber pulp board into a citric acid aqueous solution to carry out acid hydrolysis, and carrying out ultrasonic and centrifugal treatment to prepare a cellulose nanocrystal; and preparing a cellulose nanofiber filament from remaining solid fibers by using a high-pressure homogenizer. The method disclosed by the invention is green, nontoxic, short in time consumption, low in risks in a preparation process and relatively high in yield, used citric acid is easy to recycle, and therefore, the preparation cost of the nanocellulose is greatly reduced. In addition, the prepared cellulose nanocrystal and the cellulose nanofiber filament have relatively high dispersion stability, excellent specific surface area and relatively high carboxyl group content, and more chemical approaches are provided for further modification of the nanocellulose. Finally, the prepared nanocellulose has no toxic and harmful substance residues so as to have a wide application prospect on the aspect of a functional material taking the cellulose as a substrate and in particular the aspect of a material relevant to the health of a human body.

Description

technical field [0001] The invention belongs to the field of green preparation of nanocellulose, and particularly relates to a method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis combined with ultrasonic assistance. Background technique [0002] Cellulose is the most abundant renewable resource on earth, and it is also the most abundant natural polymer compound in nature. It widely exists in the cell walls of various plants, algae, fungi, etc. With the advantages of regeneration, low cost and easy modification, it is expected to replace petroleum as the main raw material of energy and chemical industry in the world in the future. [0003] Nanocellulose refers to cellulose with a diameter of 1 to 100 nm. According to the size and morphology, it can be divided into cellulose nanocrystals and cellulose nanofibrils. Cellulose nanocrystals are short in length, and are rod-like cellulose with a length of about 100nm-300nm obtained by acid or enzyme...

Claims

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Application Information

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IPC IPC(8): C08B15/04
Inventor 宋涛戢辉熊海平罗元超
Owner SOUTH CHINA UNIV OF TECH
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