Method for preparing regenerated cellulose fiber by two-step coagulating bath process
US-8962821-B2 · Feb 24, 2015 · US
US12129574B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-12129574-B2 |
| Application number | US-202117449465-A |
| Country | US |
| Kind code | B2 |
| Filing date | Sep 30, 2021 |
| Priority date | Sep 30, 2021 |
| Publication date | Oct 29, 2024 |
| Grant date | Oct 29, 2024 |
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The present disclosure relates to methods for producing functional regenerated cellulose composite fibers and products thereof. The methods can be conducted with the use of recycled and/or virgin cellulose powder.
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What is claimed is: 1. A method of preparing a regenerated cellulose composite fiber, the method comprising: providing a cellulose solution consisting of a metal hydroxide, urea, zinc oxide, cellulose having an average degree of polymerization (DP) of 300-800, and water, wherein the metal hydroxide urea, and zinc oxide are preset in cellulose solution at a concentration of 6-8% w/w, 12-14% w/w, and 0.11-0.13% w/w, respectively; filtering the cellulose solution through at least one filter thereby forming a filtered cellulose solution; combining the filtered cellulose solution with a dispersion comprising cellulose nanoparticles and water thereby forming a crude cellulose dope; filtering the crude cellulose dope through at least one filter thereby forming a filtered cellulose dope; degassing the filtered cellulose dope thereby forming a cellulose dope; and extruding the cellulose dope in a coagulation bath thereby forming the regenerated cellulose composite fiber. 2. The method of claim 1 , wherein the method further comprises combining cellulose with an aqueous solution comprising metal hydroxide, urea, zinc oxide and water, thereby forming a cellulose solution precursor; adjusting the temperature of the cellulose solution precursor to between −20° C. to 0° C.; and adjusting the temperature of the cellulose solution precursor to 0° C. to 22° C. resulting in dissolution of substantially all of the cellulose and forming the cellulose solution. 3. The method of claim 1 , wherein the step of filtering the cellulose solution comprises filtering the cellulose solution with at least one filter having a pore size of at least 5 μm. 4. The method of claim 1 , wherein the cellulose nanoparticles have an average diameter of 100-500 nm. 5. The method of claim 1 , wherein the cellulose comprises virgin or recycled cellulose having a DP of 400-800 and cellulose powder having a DP of 100-150. 6. The method of claim 5 , wherein the cellulose powder is produced by hydrothermal treatment of a cellulose powder precursor selected from the group consisting of textile waste, a virgin textile, raw cellulose material, and mixtures thereof. 7. The method of claim 6 , wherein the hydrothermal treatment comprises heating the cellulose powder precursor at a temperature between 110-150° C. under autogenic pressure in the presence of an acid. 8. The method of claim 1 , wherein the cellulose has an average DP of 400-500. 9. The method of claim 1 , wherein the metal hydroxide is an alkaline earth metal hydroxide, an alkali metal hydroxide, or a mixture thereof. 10. The method of claim 1 , wherein the metal hydroxide is sodium hydroxide. 11. The method of claim 1 , wherein the dispersion comprises the cellulose nanoparticles at a concentration of 5-15% w/w. 12. The method of claim 11 , wherein the dispersion has a pH of 11-13. 13. The method of claim 1 , wherein the method further comprises providing cellulose powder having an average particle size between 50 to 100 μm and reducing the average particle size of the cellulose powder by acid hydrolysis or mechanical grinding thereby forming the cellulose nanoparticles, wherein the cellulose nanoparticles have an average diameter of 100-500 nm. 14. The method of claim 1 , wherein the method comprises: combining cellulose having an average DP of 400-500, wherein the cellulose consists of virgin or recycled cellulose having a DP of 450-550 and cellulose powder having a DP of 100-150 with an aqueous solution consisting of sodium hydroxide, urea, zinc oxide, and water thereby forming a cellulose solution precursor, wherein the sodium hydroxide, the urea, and the zinc oxide have a concentration of 6-8% w/w, 12-14% w/w, and 0.11-0.13% w/w in the cellulose solution, respectively; adjusting the temperature of the cellulose solution precursor to between −20° C. to 0° C.; and adjusting the temperature of the cellulose solution precursor to 0° C. to 22° C. resulting in dissolution of substantially all of the cellulose and forming the crude cellulose dope; optionally filtering the crude cellulose dope with at least one filter having a pore size of 20-500 μm thereby forming a pre-filtered cellulose dope; filtering the crude cellulose dope or the pre-filtered cellulose dope with a filter having a pore size of 5 μm thereby forming a filtered cellulose dope; degassing the filtered cellulose dope under reduced pressure at a temperature between 0-20° C. thereby forming a cellulose dope; and extruding the cellulose dope in a coagulation bath thereby forming the regenerated cellulose composite fiber.
Other agents for modifying properties · CPC title
made from cellulose solutions · CPC title
Manufacture or treatment of nanostructures · CPC title
Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title
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