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Method for preparing cellulose nanowhiskers by microcrystalline cellulose through combination of alkali treatment and high intensity ultrasound

A technology of microcrystalline cellulose and nano-whisker, which is applied in the field of nano-material preparation, can solve the problems of sulfonic acid group reducing the thermal stability of cellulose nano-whisker, large consumption of cellulose nano-whisker, secondary pollution and the like , to achieve the effect of good dispersion, low cost and easy operation

Active Publication Date: 2017-02-08
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem mainly solved by the present invention: in view of the current concentrated acid hydrolysis method to prepare cellulose nano-whiskers acid consumption is large, easy to cause secondary pollution, and the remaining sulfonic acid groups reduce the thermal stability of cellulose nano-whiskers, etc., Provided is a method of using microcrystalline cellulose as a raw material, soaking, alkali treatment, acid treatment, and then combining with high-power ultrasonic to prepare cellulose nano whiskers

Method used

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  • Method for preparing cellulose nanowhiskers by microcrystalline cellulose through combination of alkali treatment and high intensity ultrasound
  • Method for preparing cellulose nanowhiskers by microcrystalline cellulose through combination of alkali treatment and high intensity ultrasound
  • Method for preparing cellulose nanowhiskers by microcrystalline cellulose through combination of alkali treatment and high intensity ultrasound

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Experimental program
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Effect test

Embodiment 1

[0039] 1) Soaking: Add microcrystalline cellulose to water and soak for 12-24 hours to obtain water-soaked microcrystalline cellulose.

[0040] 2) Alkali treatment:

[0041] According to the mass ratio of 1:10~30, add the soaked microcrystalline cellulose into the sodium hydroxide aqueous solution, keep the temperature at 70℃, and react for 1~2h under the condition of 200~2000rpm (revolution / min) to obtain the alkali-treated microbe The concentration of crystalline cellulose and sodium hydroxide aqueous solution is 3% to 5%.

[0042] 3) Acid treatment:

[0043] According to the mass ratio of 1:10-30, add alkali-treated microcrystalline cellulose to the hydrochloric acid aqueous solution, keep the temperature at 90℃, and react for 1 to 4 hours under the conditions of 200-2000rpm stirring speed to obtain acid-treated microcrystalline cellulose. The concentration of the hydrochloric acid aqueous solution It is 1% to 2%. See the SEM picture of microcrystalline cellulose after acid treat...

Embodiment 2

[0049] The difference between this embodiment and the first embodiment is:

[0050] In step 2), the reaction temperature is 80°C and the concentration of the aqueous sodium hydroxide solution is 5% to 7%;

[0051] In step 3), the reaction temperature is 85°C, and the concentration of the aqueous hydrochloric acid solution is 2% to 4%;

[0052] In step 4), the ultrasound output power is 1000-1200W, and the ultrasound time is 25-35min.

[0053] See the TEM picture of the obtained cellulose nanowhisker Figure II .

Embodiment 3

[0055] The difference between this embodiment and specific embodiments one and two is:

[0056] In step 2), the reaction temperature is 90°C and the concentration of the aqueous sodium hydroxide solution is 7%-9%;

[0057] In step 3), the reaction temperature is 80°C, and the concentration of the aqueous hydrochloric acid solution is 4% to 6%;

[0058] In step 4), the ultrasound output power is 1200~1500W, and the ultrasound time is 20~30min.

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Abstract

The invention provides a method for preparing cellulose nanowhiskers by microcrystalline cellulose through combination of alkali treatment and high intensity ultrasound. The method comprises the steps of immersion, alkali treatment, acid treatment, high intensity ultrasound processing, and freeze drying. Under prerequisite that the cellulose nanowhiskers keep type I, the method firstly and creatively uses alkali treatment and low-concentration acid treatment, high intensity ultrasound is combined to prepare the cellulose nanowhiskers, so that problems of environment pollution as well as resource and time wasting due to high-concentration strong acid processing in a traditional mode can be avoided. The prepared cellulose nanowhiskers have the advantages that dispersibility and stability are good, operation is simple, and massive concentrated acid consumption is not required, and secondary pollution cannot be generated on the environment. The crystallization degree of the cellulose nanowhiskers is greater than or equal to 70%, the diameter is about 3-20 nm, and the length is 200-400 nm.

Description

Technical field [0001] The invention relates to a method for preparing cellulose nano-whiskers from microcrystalline cellulose, more specifically to a method for preparing cellulose nano-whiskers from microcrystalline cellulose by alkali treatment combined with high-intensity ultrasound, and belongs to nano material preparation technology field. Background technique [0002] At least one dimension is in the nanoscale range (1-100nm), or materials composed of them as basic units are called nanomaterials. Cellulose nanowhiskers are ultra-fine fibers with a diameter of less than 100nm, with unique mechanical, thermodynamic and hydrodynamic properties, and can be widely used in the field of composite materials. Its blending with polymer materials can significantly change the mechanical, optical, thermal and electrical properties of polymer materials. In addition, cellulose nanowhiskers have very broad application prospects in industrial fields such as cosmetics, food, biomedical ma...

Claims

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Application Information

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IPC IPC(8): C08B15/02C08J3/28C08L1/04
CPCC08B15/02C08J3/28C08J2301/04
Inventor 周骥平姜亚妮张琦朱兴龙赵国琦
Owner YANGZHOU UNIV