Chitin nano-fibril and preparation method thereof

A technology of nanofibrils and chitin, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of high corrosion of acid-base reagents, thick chitin nanofibrils, and different lengths of chitin. The effect of cost, richness and high aspect ratio

Active Publication Date: 2016-04-27
INST OF WOOD INDUDTRY CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the chitin nanofibrils obtained after acid-base treatment in the existing preparation process of chitin nanofibrils are relatively thi

Method used

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  • Chitin nano-fibril and preparation method thereof
  • Chitin nano-fibril and preparation method thereof
  • Chitin nano-fibril and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0043] 1. Use benzene: ethanol to extract some organic matter from industrial waste shrimp shells at a ratio of 2:1, then use glacial acetic acid to adjust the pH to 4.5 and add 1wt% NaClO 2 Bleaching at 80°C for 3 hours;

[0044] 2. The bleached shrimp shells were prepared as a 1wt% solution to obtain a 1wt% coarse chitin solution by mechanical disc grinding;

[0045] 3. Put the above solution on a magnetic stirrer and stir for 15 minutes, so that chitin is evenly dispersed in the solution;

[0046] 4. Then add TEMPO, NaBr and NaClO, the molar ratio of TEMPO:NaBr:NaClO is 0.1:1:2.5, quickly seal the container and heat it to 80°C for 2 hours, after the reaction, add ethanol 20 times NaClO (molar ratio) to stop Reaction, the solution obtained is washed to neutrality with deionized water;

[0047] 5. Add the above treated solution to NaClO 2 , heated to 40-90°C, reacted for 2 hours, then washed with deionized water until neutral

[0048] 6. Prepare the solution obtained abov...

specific Embodiment 2

[0050] 1. Clean the industrial waste shrimp skin, crush it through an 80-mesh sieve, prepare a 1wt% solution, and store it at 4°C

[0051] 2. Disc-milling the above-mentioned solution by means of mechanical disc-grinding to obtain a coarse chitin dispersion solution;

[0052] 3. Take 400ml of the above solution, stir it evenly, add TEMPO and NaBr, and then add NaClO, the molar ratio of TEMPO:NaBr:NaClO is 0.1:1:2.5, and 0.5mol / L NaOH should be used to control the concentration of the solution during the dropping process. pH=10±0.5, after the dropwise addition, seal the container and heat to 75°C under magnetic stirring, react for 80 minutes, add ethanol 10 times NaClO (molar ratio) after the reaction to terminate the reaction;

[0053] 4. Rinse the obtained solution repeatedly with deionized water to neutrality, then add 8gNaClO 2 (80%) heated to 80°C, further bleached, then washed to neutral, and stored at 4°C;

[0054] 5. Prepare the solution obtained above into a 1.5% dis...

specific Embodiment 3

[0056] 1. Extract the crab shells with benzene:ethanol at a ratio of 2:1 at 80°C for 10 hours, then use hydrochloric acid to adjust the pH to 4-5 and add 1wt% NaClO 2 Heat at 80°C for 2h;

[0057] 2. Take 400ml of the above solution, stir evenly, add 0.064g of TEMPO and 0.4g of NaBr, disperse evenly, then add 2ml of 2mol / L NaClO, use 0.5mol / L of NaOH to control the pH of the solution at 10±0.5, under magnetic stirring Heat to 75°C for 2 hours, then add 20ml of ethanol to terminate the reaction, and wash the obtained solution with deionized water until neutral;

[0058] 3. Add the solution obtained above to 8gNaClO 2 (80wt%), heated to 85°C, reacted for 2.5h, then washed to neutral with deionized water;

[0059] 4. The solution obtained above was formulated into a 1% dispersion, and then the solution was treated with high-speed shear (1800W) for 40 minutes;

[0060] 5. Treat the obtained above solution with a centrifuge at 5000rpm for 10min, take the supernatant, and 2 Ultr...

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Abstract

The invention discloses chitin nano-fibril. The chitin nano-fibril is characterized in that the diameter is smaller than or equal to 10 nm, and the chitin nano-fibril is prepared with a TEMPO oxidation method. The invention further discloses specific steps. The preparation process is simple, the technology is easy to control, a used oxidant is an environment-friendly solvent and is safe and non-toxic, an environment-friendly preparation process is realized, the cost is reduced, and the prepared chitin nano-fibril is non-toxic, has a high length-diameter ratio, is uniform in structure unit distribution and has certain mechanical strength.

Description

technical field [0001] The invention relates to a chitin nanofibril and a preparation method thereof, in particular to a chitin nanofibril with a diameter less than or equal to 10 nm, which is prepared by a TEMPO oxidation method and a preparation method thereof. Background technique [0002] Chitin is a natural biopolymer, an extremely abundant natural resource on the earth, and the only positively charged nanofiber found so far in nature, because its molecular structure contains Unsaturated cationic groups, so it has a strong adsorption effect on various negatively charged harmful substances. Chitin exists in the shells of crustaceans such as shrimp, crabs, insects, etc., the cells of lower plant fungi, algae, and cell walls of higher plants in nature. The annual biosynthesis amount reaches 100 billion tons. It is a rich Organic renewable resources. However, most of the crab shells and shrimp skins, which are the main sources of chitin, are discarded as garbage. These bi...

Claims

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Application Information

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IPC IPC(8): D01F9/00C08B37/08
CPCC08B37/003D01F9/00
Inventor 卢芸叶贵超焦立超刘波殷亚方张永刚
Owner INST OF WOOD INDUDTRY CHINESE ACAD OF FORESTRY
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