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Preparation method of nano cellulose

A technology of nanocellulose and microcrystalline cellulose, applied in the field of nanomaterials, can solve the problems of unfavorable production, complicated operation, waste of fiber raw materials, etc., and achieve the effects of simple and convenient operation, simple preparation method, and abundant sources of raw materials

Inactive Publication Date: 2015-12-23
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Oxidation of regenerated cellulose with NaClO published by Masayuki Hirota in 2009 2 catalyzedbyTEMPOandNaClOunderacid-neutralconditionsdescribed in TEMPO-NaClO 2 -The method of oxidizing cellulose with NaClO oxidation system, but this method is actually only the oxidation pretreatment of cellulose, and nano-cellulose cannot be obtained, and the reaction time is very long, generally it takes more than one day to achieve the purpose of oxidation
[0004] Patent Literature Patent No. CN102964454B discloses a method for preparing nanocellulose, wherein the method directly removes the large-sized fibers that are less than nanoscale, which reduces the yield of nanocellulose and wastes fiber raw materials
[0005] The publication number of the patent document is CN103492637A, which discloses a mechanical method to prepare nanocellulose, wherein the method needs to go through several times of fine grinding and separation, and the operation is relatively complicated, which is not conducive to production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for preparing nanocellulose, comprising the following steps:

[0022] a. Disperse 2g of microcrystalline cellulose in a buffer solution prepared by 200ml of acetic acid and sodium acetate with a pH of 3.6 and a concentration of 1mol / L, and then add 2,2,6,6-tetramethylpiperidine-nitrogen oxide TEMPO0.03g, NaClO5mmol, NaClO 2 Put 0.22g in the buffer solution to obtain the reaction solution, put the reaction solution into a three-necked flask, fix the flask in the ultrasonic cleaner with an iron stand, adjust the ultrasonic power of the ultrasonic cleaner to 300w and stir the reaction with a stirrer 0.5h, add absolute ethanol until the reaction is terminated, pour it into a container and let it stand;

[0023] b. Take the lower sediment in the container of step a and wash it with 40% ethanol by volume to obtain a cellulose solution; centrifuge the cellulose solution for 3 times, take the precipitate and wash it with deionized water for 3 times, and then centrifug...

Embodiment 2

[0028] A method for preparing nanocellulose, comprising the following steps:

[0029] a. Disperse 3g of microcrystalline cellulose in a buffer solution prepared by acetic acid and sodium acetate with a pH of 5.6 and a concentration of 1.2mol / L and 400ml, and then add 2,2,6,6-tetramethylpiperidine-nitrogen Oxide TEMPO0.1g, NaClO10mmol, NaClO 2 Put 0.11g in the buffer solution to obtain the reaction solution, put the reaction solution into a three-necked flask, fix the flask in the ultrasonic cleaner with an iron stand, adjust the ultrasonic power of the ultrasonic cleaner to 350w and stir the reaction with a stirrer 1.5h, add absolute ethanol to terminate the reaction, pour it into a container and let it stand;

[0030] b. Wash the lower precipitate in the container of step a with 50% by volume ethanol to obtain a cellulose solution; centrifuge the cellulose solution for 3 times, wash the precipitate with deionized water for 3 times, and centrifuge to obtain the last separatio...

Embodiment 3

[0034] A method for preparing nanocellulose, comprising the following steps:

[0035] a. Take 5g microcrystalline cellulose and disperse it in the buffer solution prepared by pH 4, concentration 1.1mol / L, 500ml acetic acid and sodium acetate, then add 2,2,6,6-tetramethylpiperidine-nitrogen oxide TEMPO0.31g, NaClO8mmol, NaClO 2 Put 2.26g in the buffer solution to obtain the reaction solution, put the reaction solution into a three-necked flask, fix the flask in the ultrasonic cleaner with an iron stand, adjust the ultrasonic power of the ultrasonic cleaner to 500w and stir the reaction with a stirrer 2h, add absolute ethanol to terminate the reaction, pour it into a container and let it stand;

[0036] b. Take the lower precipitate in the container of step a and wash it with 60% ethanol by volume to obtain a cellulose solution; centrifuge the cellulose solution twice, take the precipitate and wash it twice with deionized water, then centrifuge, and separate the last time to ob...

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Abstract

The invention discloses a preparation method of nano cellulose. The method comprises the following steps: under an ultrasonic condition, processing microcrystalline cellulose by a TEMPO-NaClO-NaClO2 oxidization system, washing the obtained cellulose solution, subjecting the cellulosed solution to centrifugation, directly freeze-drying the upper layer suspension, subjecting the lower layer precipitate to a nano-crystallization treatment to obtain nano cellulose dispersion liquid, and freeze-drying the dispersion liquid to obtain nano cellulose. The preparation method has the advantages that the reaction time is reduced due to the ultrasonic treatment, moreover, the consumption amount of reagents is reduced, the acid / alkali treatment is eliminated, thus the length of cellulose will not be destroyed by the acid / alkali treatment, nano cellulose with large strength can be obtained, the cellulose that has not reach the nano grade is subjected to a nano-crystallization treatment to increase the raw material utilization rate, the waste is reduced, and the energy is saved.

Description

technical field [0001] The invention relates to a method for preparing nano-cellulose, which belongs to the field of nano-materials. Background technique [0002] As a nanomaterial, nanocellulose not only has the properties of nanoparticles, but also has biocompatibility. Therefore, nanofibers are studied in the fields of medicine, daily necessities, and electronics. Nanocellulose can also be used in reinforcing agents of composite materials, drug carriers, ultrafiltration materials, high barrier packaging materials, food additives and cosmetic additives, etc., so it has great research value. [0003] Oxidation of regenerated cellulose with NaClO published by Masayuki Hirota in 2009 2 catalyzedbyTEMPOandNaClOunderacid-neutralconditionsdescribed in TEMPO-NaClO 2 -The method of oxidizing cellulose with NaClO oxidation system, but this method is actually only an oxidation pretreatment of cellulose, and nano-cellulose cannot be obtained, and the reaction time is very long, and...

Claims

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Application Information

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IPC IPC(8): C08B15/02
Inventor 史昌蓉
Owner GUANGXI UNIV
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