Methods for producing ultrafine fiber and ultrafine fiber-containing sheet, sheet obtained thereby, and resin composite comprising laminated resins
US-10273633-B2 · Apr 30, 2019 · US
US11111631B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11111631-B2 |
| Application number | US-202016814501-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 10, 2020 |
| Priority date | Mar 31, 2016 |
| Publication date | Sep 7, 2021 |
| Grant date | Sep 7, 2021 |
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It is an object of the present invention to provide a method for producing ultrafine fibrous cellulose, which is capable of efficiently obtaining ultrafine fibrous cellulose having phosphoric acid groups with a high yield. The present invention relates to a method for producing fibrous cellulose having a fiber width of 1000 nm or less, comprising: a (A) of introducing phosphoric acid groups into cellulose fibers to form crosslinked structures via the phosphoric acid groups, thereby obtaining crosslinked phosphorylated cellulose fibers, a (B) of breaking some or all of the crosslinked structures to obtain crosslink-broken phosphorylated cellulose fibers, and a (C) of performing a mechanical treatment on the crosslink-broken phosphorylated cellulose fibers to obtain fibrous cellulose having a fiber width of 1000 nm or less, wherein, in the (A), crosslinked structures in an amount of 0.05 mmol/g or more and 2.0 mmol/g or less are formed, and the (B) is a step of performing the hydrolysis of the crosslinked structures in an aqueous solvent with pH 3 or more.
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The invention claimed is: 1. A method for producing fibrous cellulose having a fiber width of 1000 nm or less, comprising: (A) introducing phosphoric acid groups into cellulose fibers to form crosslinked structures via the phosphoric acid groups, so as to obtain crosslinked phosphorylated cellulose fibers, (B) breaking some or all of the crosslinked structures to obtain crosslink-broken phosphorylated cellulose fibers, and (C) performing a mechanical treatment on the crosslink-broken phosphorylated cellulose fibers to obtain fibrous cellulose having a fiber width of 1000 nm or less, wherein in the step (A), crosslinked structures in an amount of 0.05 mmol/g or more and 2.0 mmol/g or less are formed, in the step (B), 50 mol % or more of the crosslinked structures are broken, and the step (B) is performing the hydrolysis of the crosslinked structures in an aqueous solvent with pH 3 or more. 2. The method for producing fibrous cellulose according to claim 1 , wherein the step (B) is a hot alkaline treatment. 3. The method for producing fibrous cellulose according to claim 1 , wherein when the polymerization degree of the cellulose fibers before subjected to the step (A) is defined as DPa and the polymerization degree of the crosslink-broken phosphorylated cellulose fibers obtained in the step (B) is defined as DPb, the DPb/DPa value is 0.65 or more and 0.94 or less. 4. The method for producing fibrous cellulose according to claim 1 , wherein the polymerization degree (DPb) of the crosslink-broken phosphorylated cellulose fibers obtained in the step (B) is 600 or more. 5. The method for producing fibrous cellulose according to claim 1 , wherein the polymerization degree (DPc) of the fibrous cellulose having a fiber width of 1000 nm or less obtained in the step (C) is 390 or more.
Preparation of cellulose esters of inorganic acids {, e.g. phosphates (rendering cellulose suitable for esterification C08B1/02)} · CPC title
characterised by configuration · CPC title
Crosslinking of cellulose derivatives · CPC title
Crosslinking of cellulose · CPC title
Highly hydrated, swollen or fibrillatable fibres · CPC title
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