Method for producing carboxymethylated cellulose and carboxymethylated cellulose nanofibers

Patent metadata

Field	Value
Publication number	US-11518820-B2
Application number	US-201816768939-A
Country	US
Kind code	B2
Filing date	Dec 5, 2018
Priority date	Dec 7, 2017
Publication date	Dec 6, 2022
Grant date	Dec 6, 2022

Abstract

The present invention provides a novel method for producing carboxymethylated cellulose, the method making it possible to economically obtain a high-transparency cellulose nanofiber dispersion. In the carboxymethylation of cellulose, mercerization is carried out in a solvent comprising mainly water, and then carboxymethylation is carried out in a mixed solvent of water and an organic solvent. A nanofiber dispersion of high-transparency carboxymethylated cellulose can be obtained by defibrating the resulting carboxymethylated cellulose.

First claim

The invention claimed is:

1. A method for producing carboxymethylated cellulose, the method comprising:
treating cellulose with a mercerizing agent to prepare mercerized cellulose, and
reacting the mercerized cellulose with a carboxymethylation agent to produce carboxymethylated cellulose, wherein
preparing mercerized cellulose is performed in a solvent containing 70% by mass or more of water, and producing carboxymethylated cellulose is performed in a mixed solvent of water and an organic solvent;
the mixed solvent is a solvent comprising 50% by mass or more of the organic solvent;
the carboxymethylated cellulose has a degree of carboxymethyl substitution per anhydrous glucose unit of less than 0.50, and has a degree of crystallization of cellulose I type of 50% or more.

2. The method according to claim 1 , wherein the solvent containing water in preparing mercerized cellulose is a solvent containing 90% by mass or more of water.

3. The method according to claim 2 , wherein the solvent containing water in preparing mercerized cellulose is water.

4. The method according to claim 3 , wherein a rate of effective utilization of the carboxymethylation agent is 15% or more.

5. The method according to claim 4 , wherein the mercerizing agent comprises sodium hydroxide, lithium hydroxide, potassium hydroxide, or a combination of two or more thereof.

6. The method according to claim 5 , wherein the carboxymethylation agent comprises monochloroacetic acid or sodium monochloroacetate.

7. The method according to claim 6 , wherein the mixed solvent in producing the carboxymethylated cellulose is a solvent comprising 50 to 99% by mass of an organic solvent.

8. The method according to claim 7 , wherein the organic solvent comprises isopropanol, methanol, ethanol, acetone, or a combination of two or more thereof.

9. The method according to claim 8 , wherein a degree of carboxymethyl substitution per anhydrous glucose unit in the carboxymethylated cellulose is less than 0.40.

10. The method according to claim 9 , wherein a degree of crystallization of cellulose I type in the carboxymethylated cellulose is 60% or more.

11. The method according to claim 1 , wherein a rate of effective utilization of the carboxymethylation agent is 15% or more.

12. The method according to claim 1 , wherein the mercerizing agent comprises sodium hydroxide, lithium hydroxide, potassium hydroxide, or a combination of two or more thereof.

13. The method according to claim 1 , wherein the carboxymethylation agent comprises monochloroacetic acid or sodium monochloroacetate.

14. The method according to claim 1 , wherein the mixed solvent in producing the carboxymethylated cellulose is a solvent comprising 50 to 99% by mass of the organic solvent.

15. The method according to claim 1 , wherein the organic solvent comprises isopropanol, methanol, ethanol, acetone, or a combination of two or more thereof.

16. The method according to claim 1 , wherein a degree of carboxymethyl substitution per anhydrous glucose unit in the carboxymethylated cellulose is less than 0.40.

17. The method according to claim 1 , wherein a degree of crystallization of cellulose I type in the carboxymethylated cellulose is 60% or more.

18. The method according to claim 1 , wherein the step of preparing mercerized cellulose is performed in a reactor, and wherein the method further comprises adding an organic solvent or an aqueous solution of an organic solvent to the reactor before, at the same time as, or immediately after the addition of the carboxymethylation agent.

Assignees

• Jujo Paper Co Ltd

Inventors

• Inoue Kazuhiko
• Nakatani Takeshi
• Tada Yusuke

Classifications

• D21C9/007

  by mechanical or physical means · CPC title

• D06M11/40

  combined with, or in absence of, mechanical tension, e.g. slack mercerising · CPC title

• D06M13/21

  Halogenated carboxylic acids; Anhydrides, halides or salts thereof · CPC title

• C08B11/20

  Post-etherification treatments of chemical or physical type, {e.g. mixed etherification in two steps}, including purification · CPC title

• D06M2101/06

  cellulosic · CPC title