Method for preparing cellulose nanofibrils with surfaces containing carboxyls and quaternary ammonium groups

A technology of nanofibrils and cellulose is applied in the field of preparation of natural polymer materials to achieve superior gel-like properties, reduced energy consumption and significant thickening effects.

Inactive Publication Date: 2019-07-30
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pretreatment of cellulose pulp with the currently known deep eutectic solvent system, followed by mechanical treatment, can only obta

Method used

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  • Method for preparing cellulose nanofibrils with surfaces containing carboxyls and quaternary ammonium groups

Examples

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Effect test

Embodiment 1

[0027] Stir 49g of anhydrous oxalic acid and 40g of anhydrous betaine at 90°C for 5min to form a eutectic system, then add 2g of bleached hardwood pulp to the system, continue to react at 90°C for 5h, and add 100g of distilled water at 70°C, and let stand at room temperature for 5 minutes to swell the fibers. Add 200g of 80°C distilled water for dilution, then centrifuge at 6000r / min for 5min, pour out the supernatant and keep the precipitate, disperse the obtained precipitate with 400g of distilled water, and then centrifuge at 6000r / min for 5min. Repeat this centrifugation washing process with distilled water 4 times. Add 100g of distilled water to the precipitate obtained after washing to obtain a pretreated concentration of 2% cellulose solution, which is subjected to high-pressure homogenization mechanical treatment, and the homogeneous pressure used in the high-pressure homogenization process is 700bar. The number of homogenization cycles is 4 times to obtain a cellulos...

Embodiment 2

[0030] Stir 74g of anhydrous oxalic acid and 40g of anhydrous betaine at 110°C for 10 minutes to form a eutectic system, then add 5g of bleached softwood pulp to the system, continue to react at 110°C for 2 hours, and add 200g of distilled water at 70°C, and stand at room temperature for 10 minutes to swell the fibers. Add 700g of 95°C distilled water for dilution, then centrifuge at 6000r / min for 5min, pour out the supernatant and keep the precipitate, disperse the obtained precipitate with 300g of distilled water, and then centrifuge at 6000r / min for 5min. Repeat this centrifugation washing process with distilled water 4 times. Add 250 g of distilled water to the precipitate obtained after washing to obtain a pretreated cellulose solution with a concentration of 2%, which is subjected to high-pressure homogenization mechanical treatment, and homogenized 3 times at a homogenization pressure of 1300 bar.

[0031] The yield of the obtained cellulose nanofibrils is 80%; its par...

Embodiment 3

[0033]Stir 19g of anhydrous oxalic acid and 40g of betaine hydrochloride at 90°C for 5min to form a eutectic system, then add 1g of bleached grass pulp to the system, continue to react at 90°C for 5h, and add 50g of 70 ℃ distilled water, and stand at room temperature for 5 minutes to make the fibers swell. Add 200g of 70°C distilled water for dilution, then centrifuge at 10000r / min for 5min, pour out the supernatant and keep the precipitate, disperse the obtained precipitate with 100g of distilled water, and then centrifuge at 10000r / min for 5min. Repeat this centrifugation washing process with distilled water 6 times. Add 100g of distilled water to the precipitate obtained after washing to obtain a pretreated concentration of 1% cellulose solution, which is subjected to high-pressure homogenization mechanical treatment. The homogeneous pressure used in the high-pressure homogenization process is 1300bar. The number of homogenization cycles is 4 times to obtain a cellulose na...

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Abstract

The invention relates to a method for preparing cellulose nanofibrils with surfaces containing carboxyls and quaternary ammonium groups, and belongs to the field of preparation of natural polymer materials. The cellulose nanofibrils involved in the invention are prepared by pretreating 1-6 parts by mass of cellulose pulp through an eutectic solvent system consisting of 12-80 parts by mass of anhydrous oxalic acid and 40 parts by mass of alkaloid, and then mechanically treating the cellulose pulp, the alkaloid is any one of anhydrous betaine or hydrochloric betaine, the pretreatment time lastsfor 2 h-5 h, and the temperature is 90 DEG C-110 DEG C. By the method, preparation of the cellulose nanofibrils with the surfaces simultaneously containing the carboxyls and quaternary ammonium groupsis realized successfully, and the obtained product is stable in dispersion and has a good thickening effect.

Description

technical field [0001] The invention relates to the field of preparation of natural polymer materials, in particular to a preparation method of cellulose nanofibrils containing carboxyl groups and quaternary ammonium groups on the surface. Background technique [0002] Cellulose is the most abundant and biodegradable natural polymer material in nature. As the global emphasis on resources and environmental protection continues to increase, environmentally friendly and renewable cellulose resources have begun to be widely used in various fields. Cellulose nanofibrils are ultra-fine fibers with a diameter of less than 100nm. They have many excellent properties, such as high strength, high modulus, low thermal expansion coefficient, low density, renewable, and biodegradable. They are used in packaging, papermaking, and sewage purification. , biomedical and other fields have applications. [0003] The production methods of cellulose nanofibrils are roughly classified into mechan...

Claims

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Application Information

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IPC IPC(8): D06M13/463D06M13/192D06M101/06D06M101/04
CPCD06M13/192D06M13/463D06M2101/04D06M2101/06
Inventor 解洪祥司传领邹杨邹竹帆刘慰王慧刘坤刘华玉张筱仪李颖
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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