Method for manufacturing porous cellulose particles and porous cellulose particles

Patent metadata

Field	Value
Publication number	US-2016355662-A1
Application number	US-201615238723-A
Country	US
Kind code	A1
Filing date	Aug 17, 2016
Priority date	Mar 12, 2014
Publication date	Dec 8, 2016
Grant date	—

Abstract

Provided are a method of manufacturing porous cellulose particles, including a cellulose solution preparation step of preparing a cellulose solution by dissolving cellulose in an aqueous lithium bromide solution, a dispersion preparation step of preparing a cellulose solution dispersion by dispersing the cellulose solution in an organic dispersion medium, and a coagulation step of coagulating cellulose in the cellulose solution dispersion by cooling the cellulose solution dispersion and adding a coagulation solvent thereto such that porous particles are obtained, and porous cellulose particles obtained by the method for manufacturing porous cellulose particles.

First claim

What is claimed is:

1 . A method for manufacturing porous cellulose particles, comprising:
a cellulose solution preparation step of preparing a cellulose solution by dissolving cellulose in an aqueous lithium bromide solution; a dispersion preparation step of preparing a cellulose solution dispersion by dispersing the cellulose solution in an organic dispersion medium; and a coagulation step of coagulating cellulose in the cellulose solution dispersion by cooling the cellulose solution dispersion and adding a coagulation solvent thereto such that porous cellulose particles are obtained.

2 . The method for manufacturing porous cellulose particles according to claim 1 , further comprising:
a washing step of washing the porous cellulose particles obtained through the coagulation step.

3 . The method for manufacturing porous cellulose particles according to claim 1 , further comprising:
a cross-linking step of forming a cross-linked structure in the porous cellulose particles obtained through the coagulation step.

4 . The method for manufacturing porous cellulose particles according to claim 2 , further comprising:
a cross-linking step of forming a cross-linked structure in the porous cellulose particles obtained through the coagulation step.

5 . The method for manufacturing porous cellulose particles according to claim 4 ,
wherein the washing step is performed at at least any one of a point in time before the cross-linking step or a point in time after the cross-linking step.

6 . The method for manufacturing porous cellulose particles according to claim 5 ,
wherein the washing step is performed before the cross-linking step.

7 . The method for manufacturing porous cellulose particles according to claim 6 ,
wherein the washing step is a step of making each of the content of lithium ions and the content of bromide ions in a dry mass of 1 kg of the porous cellulose particles become equal to or less than 800 mmol.

8 . The method for manufacturing porous cellulose particles according to claim 3 ,
wherein the cross-linking step is a step of forming a cross-linked structure in the porous cellulose particles obtained through the coagulation step by using epichlorohydrin.

9 . The method for manufacturing porous cellulose particles according to claim 1 ,
wherein the content of lithium bromide in the aqueous lithium bromide solution is equal to or greater than 50% by mass and equal to or less than 70% by mass.

10 . The method for manufacturing porous cellulose particles according to claim 1 ,
wherein the content of cellulose in the cellulose solution is equal to or greater than 1% by mass and equal to or less than 15% by mass.

11 . The method for manufacturing porous cellulose particles according to claim 1 ,
wherein a cooling rate at the time of cooling the cellulose solution dispersion is equal to or greater than 0.2° C./min and equal to or less than 50° C./min.

12 . The method for manufacturing porous cellulose particles according to claim 1 , further comprising:
a freeze-drying step of freeze-drying the porous cellulose particles so as to obtain freeze-dried porous cellulose particles.

13 . Porous cellulose particles obtained by the method for manufacturing porous cellulose particles according to claim 1 .

14 . The porous cellulose particles according to claim 13 ,
wherein a modulus of elasticity of the porous cellulose particles calculated from a load at the time when the porous cellulose particles has a 5% strain measured by a microhardness tester is equal to or greater than 8 MPa.

15 . The porous cellulose particles according to claim 13 ,
wherein an average pore size of the freeze-dried porous cellulose particles measured by mercury intrusion porosimetry is equal to or greater than 10 nm and equal to or less than 2,000 nm.

16 . The porous cellulose particles according to claim 13 ,
wherein a specific surface area of the freeze-dried porous cellulose particles measured by mercury intrusion porosimetry is equal to or greater than 140 m 2 /g.

17 . The porous cellulose particles according to claim 13 that has a volume average particle size of equal to or greater than 1 μm and equal to or less than 2,000 μm.

18 . The porous cellulose particles according to claim 13 ,
wherein the content of lithium ions in 1 kg of dry particles obtained by drying the porous cellulose particles is equal to or greater than 0.0001 mmol and equal to or less than 100 mmol.

19 . The porous cellulose particles according to claim 13 ,
wherein the content of bromide ions in 1 kg of dry particles obtained by drying the porous cellulose particles is equal to or greater than 0.0001 mmol and equal to or less than 100 mmol.

Assignees

• Fujifilm Corp

Inventors

• Tokuoka Shinsuke
• Hori Ritsuko

Classifications

• C08J2201/0546

  the non-solvent being organic · CPC title

• C08J2301/02

  Cellulose; Modified cellulose · CPC title

• C08B1/003

  Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids (solutions used in the manufacture of monocomponent artificial filaments or cellulose or derivatives thereof D01F2/02) · CPC title

• C08B16/00

  Regeneration of cellulose · CPC title

• C08J9/28 Primary

  by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum · CPC title