Preparation method of aqueous solution redispersible cellulose nanofibers

A technology of nanofibrils and aqueous solutions, applied in the field of cellulose, can solve the problems of inability to effectively maintain the original performance and pollute the environment, and achieve the effects of universality, simple operation method and high yield.

Active Publication Date: 2019-09-24
QILU UNIV OF TECH
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Problems solved by technology

These reagents not only have a certain change and influence on the properties of CNF itself, but cannot effectively maintain its original performance, and will pollute the environment

Method used

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  • Preparation method of aqueous solution redispersible cellulose nanofibers
  • Preparation method of aqueous solution redispersible cellulose nanofibers
  • Preparation method of aqueous solution redispersible cellulose nanofibers

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preparation example Construction

[0035] As introduced in the background art, the existing aqueous solution redispersible cellulose nanofibrils preparation technology will lead to the problem that the cellulose nanofibrils are modified to varying degrees and it is difficult to maintain the original properties. Therefore, the present invention proposes a method for preparing aqueous solution redispersible cellulose nanofibrils (CNF). Take the following steps:

[0036] (1) Beating treatment: the pulp decomposed by the fiber dissociation device is beaten by a beater.

[0037] (2) Nano-homogenization: after the slurry has been processed by the beater, at room temperature, it is first processed through a 200 μm chamber, and then passed through the 200 μm and 87 μm chambers for homogenization.

[0038] (3) pH adjustment: adjust the pH of the CNF suspension to be acidic with hydrochloric acid solution, and then adjust to alkaline with sodium hydroxide solution.

[0039] (4) Add potassium chloride: weigh a certain a...

Embodiment 1

[0064] 1. Beating treatment, the pulp decomposed by the fiber disintegrator is put into the Valli beater at a pulp concentration of 10% and beat until the CSF is 100mL.

[0065] 2. For nano homogenization treatment, use a high-pressure micro-jet nano homogenizer. The processing conditions were: 10 passes through a 200 μm chamber at 200 bar, and then 15 passes through a 200 μm and 87 μm chamber at 1200 bar.

[0066] 3. pH adjustment, first adjust the pH of the CNF suspension to 3 with hydrochloric acid, then drop sodium hydroxide to adjust the pH to 8.

[0067] 4. Add potassium chloride to the CNF suspension and maintain the ionic strength at 10 mM.

[0068] 5. Drying treatment, using a vacuum drying oven to dry. Treatment conditions: -15bar, dry at 60°C for 2 days (see attachment for scanning electron microscope Figure 4 ).

[0069] 6. Redispersion, the dispersion conditions are: CNF 1%, shearing at 10000rpm for 15s. (SEM see attached Figure 5 ).

[0070] The redisper...

Embodiment 2

[0072] 1. Beating treatment, the pulp decomposed by the fiber disintegrator is put into the Valli beater with a pulp concentration of 20% to beat until the CSF is 50mL.

[0073] 2. For nano homogenization treatment, use a high-pressure micro-jet nano homogenizer. The processing conditions were: 15 passes through a 200 μm chamber at 300 bar, and then 25 passes through a 200 μm and 87 μm chamber at 1000 bar.

[0074] 3. pH adjustment, first adjust the pH of the CNF suspension to 4 with hydrochloric acid, then drop sodium hydroxide to adjust the pH to 8.

[0075] 4. Add potassium chloride to the CNF suspension and maintain the ionic strength at 15 mM.

[0076] 5. Drying treatment, drying in a vacuum oven. Treatment conditions: -10bar, 3 days drying at 55°C.

[0077] 6. Redispersion, the dispersion conditions are: CNF 0.5%, shearing at 11000rpm for 30s.

[0078] The redispersed particle diameter that this example makes is 1100~1990nm (see attached figure 2 ), the TSI is 0.0-...

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Abstract

The invention relates to a preparation method of aqueous solution redispersible cellulose nanofibers (CNF). The method comprises the following steps: firstly, performing beating treatment on a plant fiber raw material, performing nano homogenization treatment on the slurry to obtain a CNF suspension, adjusting the pH of the prepared CNF suspension, adding a certain amount of potassium chloride, and performing drying treatment. In the method provided by the invention, the CNF is prepared by adopting the mechanical method, and the yield is higher; in the method, the CNF suspension obtained after the pH is adjusted and a salt is added for treatment is easily redispersible in an aqueous solution after being dried by vacuum, and the characteristics such as stability after re-dispersion are good; the method can reduce the storage and transportation costs of the cellulose nanofibers, and is easy to operate, and suitable for large-scale production; and the method provides a novel idea and a novel method for high-value utilization of cellulose, and provides a novel method for obtaining and preparation of the aqueous solution redispersible CNF.

Description

technical field [0001] The invention belongs to the field of cellulose, and in particular relates to the preparation, drying and aqueous solution redispersion methods of nanometer cellulose. Background technique [0002] Cellulose is an abundant, renewable and biodegradable natural polymer, which has great application prospects in the production of household chemicals and papermaking, food, printing, cosmetics, oil well drilling, pharmaceuticals and other industries. At the same time, cellulose nanofibrils (CNF) have very broad application prospects due to their nanoscale, high specific surface area, high aspect ratio, low density, renewability and degradability. However, due to the high specific surface area of ​​CNF and the large number of hydroxyl groups on its surface, it leads to the irreversible agglomeration of CNF (film or powder) in the non-polar matrix during the drying process and the agglomeration of CNF (film or powder) in the composite process; The formation o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02C08J3/03C08L1/04
CPCC08B15/02C08J3/03C08J2301/04C08B1/003C08B15/08
Inventor 杨桂花马光瑞和铭陈嘉川吉兴香李伟栋
Owner QILU UNIV OF TECH
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