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Nanocrystalline cellulose preparation method

A technology of nanocellulose and cellulase, which is applied in fermentation and other directions, can solve the problems of large nanocellulose crystal particle size, high energy consumption for high-pressure homogenization, uncontrollable particle size, etc., and achieve good thermal stability and low energy consumption. The effect of low and high crystallinity

Active Publication Date: 2016-05-25
QINGDAO AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, high-pressure homogenization consumes a lot of energy
Moreover, the above methods generally have problems such as large nanocellulose crystal particle size, uncontrollable particle size, and poor thermal stability.

Method used

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  • Nanocrystalline cellulose preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Accurately weigh 6g of straw cellulose into the Erlenmeyer flask, add the required amount (the total volume of the final mixture is 200mL) of acetic acid-sodium acetate buffer solution into the Erlenmeyer flask, and then add Place the cellulase solution in a shaker, adjust the temperature to 50°C, and the oscillation frequency is 126rpm, react for 72h to enzymatically hydrolyze the cellulose, and ultrasonically 30min at intervals of 12h during this period (that is, 12.5h is a cycle), the ultrasonic power is 300W, a total of 5 times of ultrasound during the whole enzymatic hydrolysis process. After the reaction, the sample was taken out, centrifuged at 10,000rpm for 20min, washed with water until the pH was 7, and a stable cellulose colloid was obtained. The colloid solution was poured into a plate and frozen at -20°C for 24h, then freeze-dried at -80°C for 48h to obtain a powder Nanocellulose crystals.

Embodiment 2

[0022] Accurately weigh 10 g of straw cellulose and put it into the Erlenmeyer flask, add the required amount (the total volume of the final mixture is 200 mL) of acetic acid-sodium acetate buffer solution into the Erlenmeyer flask, and then add Place the cellulase solution in a shaker, adjust the temperature to 55°C, and the oscillation frequency is 130rpm, react for 96 hours to enzymatically hydrolyze the cellulose, and ultrasonically 30min at intervals of 12h during this period (that is, 12.5h is a cycle), and the ultrasonic power is 320W, a total of 7 times of ultrasound during the whole enzymatic hydrolysis process. After the reaction, the sample was taken out, centrifuged at 11000rpm for 15min, washed with water until the pH was 7, and a stable cellulose colloid was obtained. The colloid solution was poured into a plate and frozen at -24°C for 20h, then freeze-dried at -85°C for 45h to obtain a powder Nanocellulose crystals.

Embodiment 3

[0024] Accurately weigh 8 g of straw cellulose and put it into an Erlenmeyer flask, add the required amount (total volume of the final mixture is 200 mL) of acetic acid-sodium acetate buffer solution into the Erlenmeyer flask, and then add Place the cellulase solution in a shaker, adjust the temperature to 45°C, and the oscillation frequency is 120rpm, react for 120h to enzymatically hydrolyze the cellulose, during which time, ultrasonic for 30min at intervals of 12h (that is, 12.5h is a cycle), the ultrasonic power is 340W, a total of 9 times of ultrasound during the whole enzymatic hydrolysis process. After the reaction, the sample was taken out, centrifuged at 12000rpm for 10min, washed with water until the pH was 7, and a stable cellulose colloid was obtained. The colloid solution was poured into a plate and frozen at -18°C for 28h, then freeze-dried at -75°C for 50h to obtain a powder Nanocellulose crystals.

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Abstract

A nanocrystalline cellulose preparation method includes steps: using an acetic acid-sodium acetate buffer solution with pH being 4.8 to prepare a cellulose solution with the concentration being 0.03-0.05g / mL, adding cellulase for enzymolysis, and performing ultrasonic treatment at intervals of 12h in the enzymolysis process, wherein the concentration of the cellulose in the solution is 10-15U / mL, and ultrasonic treatment lasts 30-60min each time; after reaction is finished, taking out a sample, separating centrifugally, centrifugally washing precipitates, freezing and drying to obtain nanocrystalline cellulose. The one-dimension rodlike nanocrystalline cellulose is prepared by combination of cellulose endonucleases and the ultrasonic physical method. The nanocrystalline cellulose preparation method has advantages of safety, avoidance of pollution, high efficiency and low energy consumption; the nanocrystalline cellulose prepared according to the method has the advantages of high yield, high crystallinity, high thermostability and small particle size.

Description

technical field [0001] The invention belongs to the technical field of biological composite materials, and in particular relates to a preparation method of nano-cellulose crystals. Background technique [0002] At present, cellulose as a reinforcing phase to improve the mechanical properties of composite materials has attracted widespread attention. Natural cellulose is difficult to disperse uniformly in the polymer matrix, resulting in poor interfacial compatibility with the matrix, thereby reducing the mechanical properties of composite materials. performance, which limits its application fields. Nanocellulose is a product that decomposes micron-sized cellulose into nano-sized structures by chemical or physical methods. At the same time, the structure of natural cellulose and some nanoparticles has high surface activity. Nanocellulose has a unique colloidal size, which can form a stable suspension in water for a long time, thereby improving its dispersion in composite mat...

Claims

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Application Information

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IPC IPC(8): C12P19/14C12P19/04
CPCC12P19/04C12P19/14
Inventor 孙庆杰熊柳崔少宁秦洋杨洁常然然
Owner QINGDAO AGRI UNIV
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