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A technology of nanocellulose and fiber raw materials, applied in the field of nanomaterials
Inactive Publication Date: 2016-03-02
QINGDAO UNIV OF SCI & TECH
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[0004] In view of the above-mentioned prior art, the purpose of the present invention is to provide a kind of nanocellulose and its preparation method, which can solve the problem of low yield of nanocellulose and high energy consumption. problem, stable, uniform and inexpensive nanocellulose can be obtained
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Embodiment 1
[0039] A preparation method of nanocellulose, comprising the following steps:
[0040] (1) Use a blender to crush 2g of cotton fibers;
[0041] (2) Take out the broken cotton fiber, soak it in 100ml distilled water together with 3g sodium chlorite for 15min, then treat it at 70°C for 40min, during this period, use glacial acetic acid to adjust the pH of the solution to keep it at 4, repeat three times to remove the fiber most of the lignin in the raw material to obtain a suspension;
[0042] (3) Place the suspension obtained in step 2 in an ice bath (0°C), and add 250ml of 85% (volume fraction) phosphoric acid to it dropwise within 20 minutes using a dropping funnel. After calculation, the molar concentration of phosphoric acid in the total solution after adding is 10.7mol / L;
[0043] (4) Place the treated suspension in an oil bath at 120°C, stir for 100 minutes, and then quickly cool down to room temperature (20-25°C);
[0044] (5) Centrifuge with a centrifuge at 4000rpm f...
Embodiment 2
[0052] The steps are the same as in Example 1, using phosphoric acid in different proportions (the volume concentration of phosphoric acid is 44%), and other preparation process conditions, parameters, and steps are exactly the same. The yield of the prepared nanocellulose is 60.7%, and the particle size is 600-1000nm, such as Figure 6 shown.
Embodiment 3
[0054] The steps are the same as in Example 1, using phosphoric acid in different proportions (the phosphoric acid volume concentration is 55%), and other preparation process conditions, parameters, and steps are exactly the same. The yield of the prepared nanocellulose is 66.56%, and the particle size is 200-600nm, such as Figure 7 shown.
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Abstract
The invention discloses a nano cellulose, and a preparation method thereof. The preparation method comprises following steps: a fiber raw material is smashed; lignin is removed with sodium chlorite; acidolysis of cellulose is carried out with phosphoric acid; an obtained material is subjected to centrifugation; and the nano cellulose is obtained via dialysis. The invention also provides the nano cellulose prepared via the preparation method. According to the preparation method, sodium chlorite is used for processing the fiber raw material; lignin is removed; acidolysis of cellulose with phosphoric acid is carried out; and the ideal nano cellulose is obtained. The preparation method is low in energy consumption; the obtained nano cellulose is convenient to disperse; size is uniform and stable; the preparation method is simple; residue acid can be washed with deionized water; and a problem of acid solution treatment is avoided.
Description
technical field [0001] The invention belongs to the technical field of nanometer materials, and relates to nanocellulose and a preparation method thereof. Background technique [0002] The preparation method of nanocellulose is usually: mixed acid hydrolysis method, through the hydrolysis of cellulose, the nanocellulose with high purity is separated. However, the post-treatment process of mixed acid is complicated, the acid solution is difficult to handle, and the operation is complicated; using N-oxygen compound as a cellulose oxidation catalyst, and then treating the raw material with sodium bromide and sodium hypochlorite can oxidize the C6 primary hydroxyl group on the cellulose surface Carboxyl, but this method takes too long to react, the production efficiency is low, the equipment requirements are high, and the energy consumption is large. [0003] Chinese invention patent 201510416403.9 provides a method for preparing nanocellulose from sunflower seed shells, whic...
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