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Carboxyl nano-cellulose and preparation method thereof

A nanocellulose and cellulose technology, applied in the field of carboxyl nanocellulose preparation, can solve problems such as low treatment efficiency in cellulose crystallization area, and achieve the effects of energy saving and environmental protection, secondary aggregation inhibition and cost reduction in the preparation method.

Pending Publication Date: 2021-08-27
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The TEMPO oxidation method is easy to operate and has mild reaction conditions. It is the most commonly used method for the preparation of carboxylated nanocellulose, but the treatment efficiency for cellulose crystallization regions is low.

Method used

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  • Carboxyl nano-cellulose and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: A kind of carboxyl nanocellulose and its preparation method

[0019] Proceed as follows:

[0020] (1) Soak 0.5% (g / mL) bacterial cellulose in pure water overnight at normal temperature and pressure, stir well and add sodium hydroxide solution to ensure that the final concentration of sodium hydroxide solution is 8% (g / mL) , continue stirring;

[0021] (2) Then add bromoacetic acid several times, stir while adding, the total amount added is 70% of the amount fraction of sodium hydroxide substance, continue to stir overnight, add hydrochloric acid solution dropwise to adjust the pH to neutral, after the reaction is terminated Desalination:

[0022] (3) Carboxylated nanocellulose can be obtained by ultrasonically treating the desalted solution.

Embodiment 2

[0023] Embodiment 2: A kind of carboxyl nanocellulose and its preparation method

[0024] Proceed as follows:

[0025] (1) Soak 2% (g / mL) microcrystalline cellulose in pure water overnight at normal temperature and pressure, stir well and add sodium hydroxide to ensure that the final concentration of sodium hydroxide solution is 12% (g / mL) ;

[0026] (2) Add chloroacetic acid in several times, the amount of the dropwise addition is 70% of the amount of the sodium hydroxide substance, stir while adding, continue to stir for 1 hour after the dropwise addition is completed, then suction filter in the polytetrafluoro funnel, and pass Wash with water several times to remove residual sodium hydroxide and chloroacetic acid on the surface of the cellulose until the conductivity is not greater than 50 μS / cm;

[0027] (3) Carboxyl nanocellulose can be obtained by ball milling.

Embodiment 3

[0028] Embodiment 3: A kind of carboxyl nanocellulose and its preparation method

[0029] Proceed as follows:

[0030] (1) Soak 0.5% (g / mL) eucalyptus pulp in pure water overnight at normal temperature and pressure, stir well and add sodium hydroxide solution to make the final concentration of sodium hydroxide solution 9% (g / mL) ;

[0031] (2) Add iodoacetic acid several times, the amount added is 50% of the amount of sodium hydroxide, continue to stir for 2 hours, add acetic acid solution dropwise to adjust the pH to neutral, and desalt after the reaction is terminated;

[0032] (3) Carboxylated nanocellulose can be obtained by ultrasonic treatment.

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Abstract

The invention relates to a carboxyl nano-cellulose and a preparation method thereof. The preparation method comprises the following steps: (1) soaking cellulose in water overnight at normal temperature and normal pressure, performing uniform stirring, and adding a sodium hydroxide solution; (2) adding a halogen-substituted carboxyl compound, performing continuous stirring, then dropwise adding an acid solution to adjust a pH value to be 7, and carrying out desalting after a reaction is ended, or directly removing the sodium hydroxide solution and the halogen-substituted carboxyl compound through suction filtration to terminate the reaction; and (3) after the reaction is ended, carrying out mechanical grinding treatment such as ultrasonic treatment and homogenization to obtain the carboxyl nano-cellulose. According to the method provided by the invention, the reaction can be carried out at room temperature, and an organic solvent does not need to be added in a reaction process, so the convention that the organic solvent needs to be added in a cellulose carboxylation process is broken, the energy consumption of nano-cellulose preparation is reduced, and the cost of environmental treatment in the nano-cellulose preparation process is saved.

Description

technical field [0001] The invention relates to a carboxy nano cellulose and a preparation method thereof, in particular to a method for preparing carboxy nano cellulose in an aqueous phase at normal temperature and pressure, and belongs to the technical field of carboxy nano cellulose preparation. Background technique [0002] Cellulose is a natural renewable resource with abundant reserves. The introduction of carboxyl groups on the surface of cellulose destroys the hydrogen bond between cellulose molecules and reduces the time and energy of mechanical treatment (ultrasonic, homogenization, etc.) during the preparation of nanocellulose. consumption; on the other hand, it provides active linking groups for the subsequent modification of the cellulose surface. The TEMPO oxidation method is easy to operate and has mild reaction conditions. It is the most commonly used method for the preparation of carboxylated nanocellulose, but the treatment efficiency for cellulose crysta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/04
CPCC08B15/04
Inventor 王晓映王守娟孔凡功
Owner QILU UNIV OF TECH
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