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Preparation method of oxidized nanocellulose

A technology of nanocellulose and cellulose, applied in the field of preparation of oxidized nanocellulose, can solve the problems of uneven oxidation of nanocellulose, insufficient environmental protection of nanocellulose, and easy to corrode equipment, etc.

Active Publication Date: 2021-04-23
水木山海科技(佛山)有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Based on this, in order to solve the problems that the preparation of nanocellulose in the prior art is not environmentally friendly, easy to corrode equipment and uneven oxidation of nanocellulose, the present invention provides a method for preparing oxidized nanocellulose. The specific technical scheme is as follows:

Method used

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  • Preparation method of oxidized nanocellulose
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  • Preparation method of oxidized nanocellulose

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preparation example Construction

[0028] A method for preparing oxidized nanocellulose in one embodiment of the present invention comprises the following steps:

[0029] breaking the cellulose raw material into pieces to obtain cellulose pieces;

[0030] Add the cellulose fragments to the aqueous solution containing citric acid, then add the polyol and sulfuric acid solution, stir evenly, raise the temperature to 95°C-100°C, and let it stand for 3h-5h to obtain the cellulose suspension;

[0031] Suction filtration of the cellulose suspension under vacuum conditions to recover citric acid to obtain cellulose pulp;

[0032] The cellulose pulp is washed with deionized water, and the pH of the cellulose pulp is adjusted to neutrality with lye;

[0033] Add water to the cellulose pulp, adjust the mass percentage of the solid content of the cellulose pulp to 1%-5%, add NaBr and TEMPO under the condition of stirring, after stirring evenly, add the NaClO solution dropwise, real-time monitoring of the precise pH , th...

Embodiment 1

[0056] A method for preparing oxidized nanocellulose, comprising the steps of:

[0057] The wood pulp board is crushed into wood pulp board fragments with a diameter and a length of less than 10mm with a pulverizer;

[0058] Wood pulp board fragments are added in the aqueous solution that mass percent content is 80% citric acid, and the quality of wood pulp board fragments accounts for 8% of the aqueous solution quality of citric acid, then adds 10% of the aqueous solution quality of citric acid Ethylene glycol, and finally add sulfuric acid solution accounting for 5% of the mass of the aqueous solution of citric acid, and the solid content of the added sulfuric acid solution is 30% by mass, stir evenly and heat up to 95°C for standing reaction for 3h to obtain a cellulose suspension ;

[0059] Suction filtration of the cellulose suspension under vacuum conditions, evaporation and recrystallization of the filtrate at room temperature or recovery of citric acid by distillation u...

Embodiment 2

[0064] A method for preparing oxidized nanocellulose, comprising the steps of:

[0065] The straw pulp board is crushed into straw pulp board fragments with a diameter and a length of less than 10 mm with a crusher;

[0066] The straw pulp board fragments are added to the aqueous solution of 65% citric acid by mass percentage content, and the quality of the straw pulp board fragments accounts for 10% of the aqueous solution quality of citric acid, and then add 1% of the aqueous solution quality of citric acid Ethylene glycol, finally add sulfuric acid solution accounting for 1% of the mass of the aqueous solution of citric acid, and the solid content of the added sulfuric acid solution is 30% by mass, stir evenly, heat up to 100°C and let stand for reaction for 5h to obtain a cellulose suspension ;

[0067] Suction filtration of the cellulose suspension under vacuum conditions, evaporation and recrystallization of the filtrate at room temperature or recovery of citric acid by...

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Abstract

The invention provides a preparation method of oxidized nanocellulose, which is characterized in that polyhydric alcohol is added, and under the catalytic action of sulfuric acid, the reaction efficiency can be guaranteed, and side reactions occurring in the reaction process can be inhibited. The preparation method disclosed by the invention is environment-friendly and relatively low in cost, and can ensure the output rate of cellulose in unit time, thereby being beneficial to reducing the production cost. Besides, a sodium hypochlorite solution is added, so that the reaction is gentle, the oxidation of the nanocellulose is more uniform, and the oxidized nanocellulose with better uniformity and quality is obtained. Generally, the problems that the prepared nanocellulose is not environmentally friendly enough, equipment is prone to corrosion, and nanocellulose oxidation is uneven in the prior art can be solved.

Description

technical field [0001] The invention relates to the field of preparation of nanocellulose, in particular to a preparation method of oxidized nanocellulose. Background technique [0002] Nanocellulose is a kind of cellulose with nanometer scale. According to different material sources, preparation methods and fiber shapes, nanocellulose can be divided into cellulose nanocrystals (CNC), cellulose nanofibrils (CNF), and bacterial synthetic nanofibers. fiber (BNC). As a new type of green nanomaterial, nanocellulose has good flexibility and mechanical properties. The fibers are interlaced with each other, and it is easy to form a porous structure that is convenient for ion and electron transmission; the surface of the fiber is also attached with hydrophilic functional groups such as hydroxyl and carboxyl groups. , has good moisturizing ability. Nanocellulose is generally a nanoscale cellulose crystal separated from fiber raw materials by chemical, physical or biological methods...

Claims

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Application Information

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IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 罗屹东王国忠李玉柱
Owner 水木山海科技(佛山)有限责任公司
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