IP Library Granted Patent US 10,144,786
Granted Patent B2
US 10,144,786 · App. 15/092,589 · Granted Dec 4, 2018

Method of making nanocrystalline cellulose

Inventors: Sherif Shawki Zaki Hindi (Jeddah, SA); Refaat Atalla Abohassan (Jeddah, SA)
Assignee: King Abdulaziz University
C08B15/00C08B15/02B05D3/00C08B1/00C08L1/02
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Quick Facts
Patent No.
US 10,144,786
App. No.
15/092,589
Granted
Dec 4, 2018
Kind
B2
Abstract

The method of making nanocrystalline cellulose is a flash lyophilized-acidic hydrolysis method for converting cellulosic fibers into nanocrystalline cellulose. Cellulosic fibers are initially ground in a high-speed, rotary grinder to produce ground cellulose fiber. The ground cellulose fiber is then dried to produce dried, ground cellulose, which is then freeze-dried to yield lyophilized cellulose. Pure concentrated sulfuric acid is then added to the lyophilized cellulose at a liquid/solid ratio of 1:1 (vol/wt) to form a cellulosic paste. The cellulosic paste is diluted in either water or absolute ethanol at a liquid/solid ratio of 1:1 (vol/wt) to form a cellulosic solution, which is then filtered under cooling by liquid nitrogen-vapor. The nanocrystalline cellulose precipitate is then washed until neutralization and dried to yield nanocrystalline cellulose.

Claims (10)

1. A method of making nanocrystalline cellulose, consisting of the sequential steps of:

grinding cellulosic fibers to produce ground cellulose fiber;

drying the ground cellulose fiber to produce dried, ground cellulose, wherein the drying is done at about 105° C. for two hours;

freeze-drying the dried, ground cellulose by exposing the dried, ground cellulose to liquid nitrogen-vapor for five minutes to produce lyophilized cellulose;

adding at least 98.06% pure sulfuric acid to the lyophilized cellulose at a liquid/solid ratio of 1:1 (vol/wt) and stirring to form a cellulosic paste;

diluting the cellulose paste in a cold liquid at a liquid/solid ratio of 1:1 (vol/wt) to form a cellulosic solution, wherein the cold liquid is selected from the group consisting of water and absolute ethanol;

filtering the cellulosic solution under cooling by liquid nitrogen-vapor to produce a nanocrystalline cellulose precipitate;

washing the nanocrystalline cellulose precipitate until neutralization, wherein the washing is performed in a liquid selected from the group consisting of cold water and ethanol; and

air-drying the washed nanocrystalline cellulose precipitate for one hour to yield a nanocrystalline cellulose product, wherein the cellulose product comprises cellulose needles configured as whiskers.

2. The method of making nanocrystalline cellulose as recited in claim 1 , wherein the step of drying the ground cellulose fiber further comprises desiccating the ground cellulose fiber.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 6, 2016
From: HINDI, SHERIF SHAWKI ZAKI, DR.; ABOHASSAN, REFAAT ATALLA, DR.
To: KING ABDULAZIZ UNIVERSITY
Reel/Frame 038211/0169 →
Continuity (1)
Related Publication 20170291962A1 · Oct 12, 2017
Cited By (2)
US 12,692,653 US 12,709,648