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Nano-crystalline cellulose fiber high in carboxyl group content and preparation and application thereof

A technology of nanocellulose and high carboxyl group, which can be applied to artificial filaments made of cellulose derivatives, processing wastewater treatment, alkali metal oxides/hydroxides, etc. The subsequent use of nanocellulose and the large loss of cellulose can achieve the effect of high carboxyl group content, increasing total carboxyl group content, and improving oxidation efficiency.

Inactive Publication Date: 2016-04-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the existing preparation methods of nanocellulose fibers mainly have the following deficiencies: the TEMPO oxidation process mainly focuses on C 6 Selective oxidation of positional hydroxyl groups, for C 2 and C 3 The oxidation of the hydroxyl group in the position is not paid attention to (there is no report in the literature), and the prepared nanocellulose contains a small amount of or even no carboxyl group (acid hydrolysis method), which is not conducive to the subsequent use of nanocellulose (the carboxyl group contained in nanocellulose is carried in water. Negative charge, the adsorption capacity of heavy metals is greatly improved), the loss of cellulose is large, and the yield of nanocellulose is low

Method used

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  • Nano-crystalline cellulose fiber high in carboxyl group content and preparation and application thereof
  • Nano-crystalline cellulose fiber high in carboxyl group content and preparation and application thereof
  • Nano-crystalline cellulose fiber high in carboxyl group content and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Take 5g of dry and bleached bamboo pulp, tear it into small pieces and disperse in 1000ml deionized water, disperse the slurry evenly with a high-speed disperser, add 7g of sodium periodate to the slurry, and then place it in a heat-collecting magnetic In the stirrer, set the temperature to 50°C and react for 0.5h to obtain the pretreated slurry. Its yield is 90.952% through sampling test.

[0034] (2) Add 700ml of 0.2M NaClO to the pretreated slurry obtained in step (1) 2 solution and 50ml of 1M acetic acid solution, mixed evenly, placed in a heat-collecting magnetic stirrer, set the temperature at 30°C, and reacted for 1h to obtain a pre-oxidized slurry. At the same time, parallel experiments were done, and the obtained pre-oxidized slurry was used to test the yield of the slurry: washed with distilled water for 3 times, wrung out, dried in vacuum -0.1Mpa, 60°C, 10h, the measured fiber yield was 75.713%, and the carboxyl content was 75.713%. It is 0.6231 mmol / g....

Embodiment 2

[0041] (1) Take 10g of absolutely dry bleached bamboo pulp, tear it into small pieces and disperse it in 1000ml deionized water, disperse the slurry evenly with a high-speed disperser, add 8.2g of sodium periodate to the slurry, and then place it in a heat collecting type In the magnetic stirrer, set the temperature to 55° C., and react for 1 hour to obtain the pretreated slurry. Its yield is 90.795% through sampling test.

[0042] (2) Add 800ml of 0.2M NaClO to the pretreated slurry obtained in step (1) 2 solution and 60ml of 1M acetic acid solution, mixed evenly, placed in a heat-collecting magnetic stirrer, set the temperature at 40°C, and reacted for 2 hours to obtain a pre-oxidized slurry. At the same time, parallel experiments were done, and the obtained pre-oxidized slurry was used to test the yield of the slurry: washed with distilled water for 3 times, wrung out, and dried in a vacuum at -0.1Mpa, 60°C, for 12 hours, the measured fiber yield was 76.232%, and the carbo...

Embodiment 3

[0047] (1) Take 15g of dry and bleached bamboo pulp, tear it into small pieces and disperse in 1000ml deionized water, disperse the slurry evenly with a high-speed disperser, add 9g of sodium periodate to the slurry, and then place it in a heat-collecting magnetic In the stirrer, set the temperature to 60° C., and react for 1.5 hours to obtain the pretreated slurry. Its yield is 90.647% through sampling test.

[0048] (2) Add 900ml of 0.2M NaClO to the pretreated slurry obtained in step (1) 2 solution and 70ml of 1M acetic acid solution, mixed evenly, placed in a heat-collecting magnetic stirrer, set the temperature at 50°C, and reacted for 3 hours to obtain a pre-oxidized slurry. At the same time, parallel experiments were done, and the obtained pre-oxidized slurry was used to test the yield of the slurry: washed with distilled water for 3 times, wrung out, dried in vacuum -0.1Mpa, 60°C, 12h, the measured fiber yield was 75.696%, and the carboxyl content was 75.696%. It is ...

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Abstract

The invention belongs to the technical field of biomass nanometer materials and discloses a nano-crystalline cellulose fiber high in carboxyl group content and preparation and application thereof. A preparation method comprises the steps of preheating fiber slurry for 0.5-1.5h with sodium periodate at the temperature of 50-60 DEG C; adding a sodium chlorite solution and acetum into the slurry to be reacted for 1-3h at the temperature of 30-50 DEG C, adding TEMPO, NaClO2 and NaClO, and performing microwave heating to the temperature of 55-65 DEG C to enable the mixture to be reacted for 1-3h; performing ultrasonic dispersion and freeze drying to obtain the nano-crystalline cellulose fiber high in carboxyl group content. According to the nano-crystalline cellulose fiber, hydroxyl at the positions of C2 and C3 of cellulose is oxidized into a formyl group which is oxidized into carboxyl by sodium chlorite, hydroxyl at the position of C6 is selectively oxidized into carboxyl through a TEMPO neutral oxidation system, and accordingly the total carboxyl group content of the fiber is greatly increased, and obtained products can be used for advanced treatment of waste water at the middle section of paper making.

Description

technical field [0001] The invention belongs to the technical field of biomass nanomaterials, and in particular relates to a nanocellulose fiber with high carboxyl group content and its preparation and application. Background technique [0002] Compared with ordinary cellulose, nanocellulose fiber has a large specific surface area, superior stable dispersion, unique three-dimensional network structure and a large number of hydroxyl groups on the surface, making nanocellulose fiber a hot and excellent load material and modification Polymer materials (SiqueiraG, et al. Polymers, 2010, 2(4):728). [0003] The existing preparation methods of nanocellulose fibers are mainly the combination of chemical pretreatment and mechanical treatment. Fiber pretreatment mainly contains enzyme pretreatment (HenrikssonM, etal.European Polymer Journal, 2007,43(8):3434~3441), neutral 2,2,6,6-tetramethylpiperidine-1-oxide (TEMPO ) Microwave catalytic oxidation (Xiang Xiudong, et al. Forest Prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/24C08B15/04B01J20/24B01J20/28C02F1/28C02F103/28
CPCB01J20/24B01J20/28023C02F1/286C02F1/288C02F2103/28C08B15/04D01F2/24
Inventor 刘玉万小芳李友明
Owner SOUTH CHINA UNIV OF TECH
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