Nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer and preparation method thereof

Patent metadata

Field	Value
Publication number	US-11760843-B2
Application number	US-202318125690-A
Country	US
Kind code	B2
Filing date	Mar 23, 2023
Priority date	Jan 6, 2021
Publication date	Sep 19, 2023
Grant date	Sep 19, 2023

Abstract

The invention provides a nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer and a preparation method thereof. In the present invention, the cotton linter pulp is pulverized into flocculent fibers, fed to sulfuric acid, and reacted. After centrifugation, dialysis and ultrasonic cell disruption, cellulose nanocrystals are obtained. Carboxylated cellulose nanocrystals are further obtained after oxidation with TEMPO, dialysis, and freeze-drying. The carboxylated nanocrystals are further added to DMF, and under a nitrogen atmosphere, glycidol is grafted to the hydroxyl groups on the surface by heating with stirring. After the reaction is completed, the product is centrifuged, dried under vacuum, dialyzed, and freeze dried to obtain a nanomaterial of primary polyglycerol grafted cellulose nanocrystals. Dendrimers with different particle size ranges can be prepared by controlling the number of reactions, which contain a large number of hydroxyl groups on the surface, and are amenable to various modifications.

First claim

What is claimed is:

1. A method for preparing a nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer, using a cotton linter pulp as a raw material,
the method comprising steps of:
(1) pulverizing cotton linter pulp into flocculent fibers, feeding to sulfuric acid, reacting, centrifuging, dialyzing, and performing ultrasonication to obtain cellulose nanocrystals;
(2) dissolving the cellulose nanocrystals into water to obtain a cellulose nanocrystal solution, oxidizing the solution with TEMPO, then dialyzing, and freeze drying to obtain carboxylated cellulose nanocrystals;
(3) adding the carboxylated cellulose nanocrystals into an organic solvent, adding glycidol dropwise with stirring and heating under a nitrogen atmosphere to graft glycidol to hydroxyl groups on the surface of the carboxylated cellulose nanocrystals, centrifuging after reaction, drying under vacuum, dialyzing, and freeze drying to obtain the nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer.

2. The method according to claim 1 , further comprising: replacing the carboxylated cellulose nanocrystals in Step (3) by the nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer obtained in Step (3), and repeating Step (3), to further obtain the nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer with various particle sizes.

3. The method according to claim 1 , wherein in Step (2), the oxidization with TEMPO comprises mixing the cellulose nanocrystal solution uniformly with tetramethyl piperidine N-oxide and sodium bromide, adding sodium hypochlorite, and reacting for 3-24 h at pH 9.8-11.2 and 25-45° C., wherein the concentration of the cellulose nanocrystal solution is 1-20 mg/ml.

4. The method according to claim 1 , wherein the oxidation rate of the carboxylated cellulose nanocrystals in Step (2) is 5-20%.

5. The method according to claim 1 , wherein in Step (1), the concentration of sulfuric acid is 25-70%, the reaction temperature is 29-70° C., the reaction time is 3-12 h, the power of ultrasonication is 30-50%, the time of ultrasonication is 4-35 min, and the supernatant is collected by centrifugation at 7000-13000 rpm/min, to obtain the cellulose nanocrystals.

6. The method according to claim 1 , wherein in Step (3), the concentration of glycidol is 10-30%, and the weight ratio of the carboxylated cellulose nanocrystals to glycidol is 1.5-1.15.

7. The method according to claim 1 , wherein in Step (3), the stirring time is 30-90 min, the speed is 300-800 rpm/min, and the temperature is 80-120° C.

8. The method according to claim 1 , wherein in Step (3), glycidol is added stepwise at a rate of 10-150 μl/min for 4-24 h.

9. The method according to claim 2 , wherein in Step (3), the particle size of the nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer is in the range of 300-1000 nm.

10. A nanomaterial of polyglycerol grafted cellulose nanocrystal dendrimer prepared by the method according to claim 1 .

Assignees

• Univ Jiangnan

Inventors

• Xu Shuqin
• Chen Jinghua
• Mao Baoliang

Classifications

• C08G83/005 Primary

  Hyperbranched macromolecules · CPC title

• C08B1/06 Primary

  Rendering cellulose suitable for etherification {(etherification per se C08B11/00)} · CPC title

• C08G83/003 Primary

  Dendrimers · CPC title

• C08G65/2615

  the other compounds containing carboxylic acid, ester or anhydride groups · CPC title

• C08L1/04

  Oxycellulose; Hydrocellulose {, e.g. microcrystalline cellulose} · CPC title