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Method for producing cellulose fine fiber

A manufacturing method and technology of microfibers, applied in post-treatment modification of cellulose pulp, modification of pulp properties, pretreatment with acidic compounds, etc., achieves the effects of less damage, excellent redispersibility, and large aspect ratio

Inactive Publication Date: 2019-04-16
FUTAMURA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, only the chemical modification process cannot be used to defibrate and requires a strong mechanical defibrillation process

Method used

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  • Method for producing cellulose fine fiber
  • Method for producing cellulose fine fiber
  • Method for producing cellulose fine fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0133] Add 10 g of formic acid aqueous solution and 0.3 g of cellulose pulp to a 20 ml sample bottle, stir with a magnetic stirrer for 3 hours, transfer to a 200 ml centrifuge tube, add 100 ml of distilled water, and wash by centrifugation. Centrifugation was performed three times in the same manner to remove formic acid and obtain cellulose fine fibers. The modification rate of the obtained cellulose fine fibers was quantified by solid-state NMR. In addition, the degree of defibration was observed with an optical microscope. The shape of the fine fiber was observed by FE-SEM. The results are shown in Table 1. As shown in Table 1, it was found that the surface of the cellulose fine fibers was not modified. The SEM photos are shown in figure 1 . The average fiber diameter of the cellulose fine fibers was 100 nm or less, and the average fiber length was 13.9 μm. The obtained fine fibers can be redispersed in water or ethylene glycol after drying at 105°C. Table 1 shows th...

Embodiment 2

[0135] Cellulose fine fibers were obtained in the same manner as in Example 1 except that 9 g of formic acid aqueous solution and 1 g of propionic anhydride were used instead of 10 g of formic acid aqueous solution, and the defibrating time was changed from 3 hours to 5 hours. The obtained cellulose fine fibers were evaluated in the same manner as in Example 1. The average ester substitution degree of the cellulose fine fibers was 0.5, the average fiber diameter was 100 nm or less which was substantially the same as in Example 1, and the average fiber length was 15.0 μm. The obtained fine fibers can be redispersed in dimethylacetamide, acetone, or methyl ethyl ketone after being dried in a blow dryer at 105°C. The SEM images of the fine fibers are shown in figure 2 . Table 1 shows the measurement results of crystallinity.

Embodiment 3

[0137] Except having used acetic anhydride instead of propionic anhydride, it carried out similarly to Example 2, and obtained the cellulose fine fiber. The obtained cellulose fine fibers were evaluated in the same manner as in Example 2. The average degree of ester substitution of the cellulose fine fibers was 0.6, the average fiber diameter was 100 nm or less, and the average fiber length was 12.2 μm. The obtained microfibers can be re-dispersed in dimethylacetamide after drying with a 105° C. blast dryer. The SEM images of the fine fibers are shown in image 3 . Table 1 shows the measurement results of crystallinity.

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Abstract

Provided is a method for producing a cellulose fine fiber that has a nano size and high crystallinity and rarely undergoes the damage of a fiber shape, by impregnating cellulose with a formic acid-containing fiberizing solution and then fiberizing the cellulose, without requiring vigorous mechanical fragmentation of the cellulose. Also provided is a method for producing a surface-modified cellulose fine fiber in which the cellulose is modified. The method for producing a cellulose fine fiber according to the present invention involves impregnating cellulose with a fiberizing solution, i.e., formic acid, a formic acid-rich aqueous solution or a solution of formic acid or a formic acid-rich aqueous solution in an aprotic solvent having a number of donors of 26 or more and then fiberizing thecellulose. The method for producing a surface-modified cellulose fine fiber according to the present invention is characterized in that the fiberizing solution further contains a modification reaction agent and the method involves impregnating cellulose with the fiberizing solution and then modifying the microfibril surface of the cellulose while fiberizing the cellulose.

Description

technical field [0001] The present invention relates to a method for producing cellulose fine fibers. Background technique [0002] Cellulose fibers (cell wall units) are aggregates of fine cellulose fibers (microfibrils). Microfibrils have mechanical properties comparable to those of steel and have nanostructures with a diameter of about 20nm. Therefore, they have attracted a lot of attention from society as reinforcing materials. However, since the fibers of the microfibers are bound by hydrogen bonds, in order to take out the microfibers, it is necessary to break the hydrogen bonds and separate the microfibrils (referred to as defibrillation). Therefore, a mechanical defibrillation method that applies severe physical force has been developed. [0003] As a method for producing cellulose nanofibers, a method of producing cellulose nanofibers by an underwater mechanical fibrillation method is known. In this method, cellulose is swollen with water, and is nano-sized by st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21H11/18C08B15/08
CPCC08B15/08D21H11/18D21H11/20D21C9/002D21C9/005C08B3/06C08B3/08D21C1/04
Inventor 林莲贞丸田彩子堀正典
Owner FUTAMURA CHEM
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