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Preparation method of dialdehyde cellulose nanowhisker

A technology of dialdehyde cellulose and nano-whiskers is applied in the field of cellulose derivatives, which can solve few problems and achieve the effects of simple method, controllable size and high yield.

Pending Publication Date: 2018-05-15
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, current researches mainly focus on the derivatization of cellulose molecules, such as cellulose dialdehyde modification, while there are few studies on the conversion of cellulose nanowhiskers into derivative forms.

Method used

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  • Preparation method of dialdehyde cellulose nanowhisker
  • Preparation method of dialdehyde cellulose nanowhisker
  • Preparation method of dialdehyde cellulose nanowhisker

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The cotton linters puree was mechanically stirred and crushed, 50 g was added to 500 mL of 30% sulfuric acid, and the mixture was stirred and reacted in a water bath at 60° C. for 6 hours. Dilute with water to terminate the reaction, wash by centrifugation at 8000 rpm for 20 min, take the precipitate, resuspend in pure water, and wash by centrifugation again. This step is repeated 3 to 4 times. The milky white suspension finally obtained was dialyzed until the pH value was neutral. The dialysis product was subjected to ultrasonic treatment with a cell disruptor, 240W, 5min, 3000rpm, 10min, and the supernatant was taken to obtain a suspension of cellulose nanowhisker CNC-1, which was stored at 4°C. The yield rate of CNC-1 is ~80% calculated by the weighing method, and the hydrodynamic radius of CNC-1 suspension (R h ) Is ~1000nm.

Embodiment 2

[0026] The cotton linters puree was mechanically stirred and crushed, and 50 g was fed into 500 mL 30% sulfuric acid, and the mixture was stirred and reacted in a water bath at 60° C. for 8 hours. Dilute with water to terminate the reaction, wash by centrifugation at 8000 rpm for 20 min, take the precipitate, add pure water to resuspend, and wash again by centrifugation. This step is repeated 3 to 4 times. The milky white suspension finally obtained was dialyzed until the pH value was neutral. The dialysis product was ultrasonically treated with a cell disruptor, 240W, 10min, centrifuged at 10000rpm, 10min, and the supernatant was taken to obtain a suspension of cellulose nanowhisker CNC-2, which was stored at 4°C. The yield of CNC-2 calculated by the weighing method was ~50%. figure 1 It shows that the DLS particle size distribution of CNC-2 is mainly a single symmetrical peak, indicating that its size is uniform, R h The value is ~255nm. figure 2 The projection electron micr...

Embodiment 3

[0028] The cotton linters puree was mechanically stirred and crushed, and 50 g was fed into 500 mL 30% sulfuric acid, and the mixture was stirred and reacted in a water bath at 60° C. for 8 hours. Dilute with water to terminate the reaction, wash by centrifugation at 8000 rpm for 20 min, take the precipitate, add pure water to resuspend, and wash again by centrifugation. This step is repeated 3 to 4 times. The milky white suspension finally obtained was dialyzed until the pH value was neutral. The dialysis product was subjected to ultrasonic treatment with a cell disruptor at 240W for 5min to obtain a suspension of cellulose nanowhiskers and stored at 4°C.

[0029] Follow NaIO 4 The mass ratio of the cellulose nano whisker is 1:1, and the strong oxidant sodium periodate (NaIO 4 ), avoid light and dissolve in pure water. Adjust the pH value of the cellulose nanowhisker suspension to 2 to 4, and preheat to 85°C. NaIO 4 The solution was slowly added dropwise to the pretreated cell...

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Abstract

The invention discloses a preparation method of a dialdehyde cellulose nanowhisker. The preparation method comprises the following steps: hydrolyzing cotton linter primary pulp with 30% sulfuric acidat 60 DEG C for 4 to 10 hours, centrifuging, washing and dialyzing; carrying out ultrasonic crushing and centrifuging to prepare the cellulose nanowhisker with controllable size and the yield up to 80percent; and carrying out dialdehyde reaction on the cellulose nanowhisker at 40 to 90 DEG C by using a strong oxidizer NaIO4 for 2 to 4 hours, and combining with the steps of ultrasonic crushing andcentrifuging to take supernatant, thus obtaining the dialdehyde cellulose nanowhisker. The size range is 100 to 900 nm, the aldehyde substitution degree is 10 to 71.2 percent and the yield is up to 60 percent. According to the preparation method of the dialdehyde cellulose nanowhisker, disclosed by the invention, the dialdehyde cellulose nanowhisker is prepared by adopting a sodium periodate method; and the sodium periodate method has the advantages of controllable aldehyde degree, controllable whisker size and high yield.

Description

Technical field [0001] The invention relates to the technical field of cellulose derivatives, in particular to a method for preparing dialdehyde-modified cellulose nano whiskers. Background technique [0002] As the most extensive biomass resource in nature, cellulose is also a natural polymer with excellent performance. Since natural cellulose mainly exists in the form of microfibers, there is a very strong intramolecular and intermolecular hydrogen bond network, which makes it extremely difficult to melt and dissolve. By carrying out different kinds of derivatization reactions on cellulose molecules, including methyl cellulose, ethyl cellulose, carboxymethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methyl cellulose, etc., it can effectively improve the fiber The solubility and processing performance of the element molecule, and its derivative form is widely used in the fields of medicine, food, energy and chemical industry. [0003] Cellulose nanowhiskers refer to n...

Claims

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Application Information

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IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 许淑琴周姝妤梁李园陈敬华
Owner JIANGNAN UNIV
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