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A kind of efficient preparation method of cellulose nanocrystal

A cellulose and nanocrystal technology, applied in the post-processing of cellulose pulp, fiber raw material processing, papermaking, etc., can solve problems such as no pretreatment steps, improve reaction accessibility, and improve acid hydrolysis reaction efficiency. , easy-to-control effects

Active Publication Date: 2019-04-09
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned various methods of preparing cellulose nanocrystals, the cellulose raw material is directly processed, and there is no pretreatment step

Method used

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  • A kind of efficient preparation method of cellulose nanocrystal
  • A kind of efficient preparation method of cellulose nanocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Break 5 grams of pulp cellulose into cotton wool with a mixer, add 250ml, 4wt% NaOH solution, soak for 24 hours, then use deionized water to filter and wash it to neutral, and take this alkali-pretreated fiber prime, add 0.078 g CuSO 4 ·5H 2 0, add 90 milliliters of 64wt% sulfuric acid again, after stirring at 50 DEG C for 40min, add deionized water to terminate the reaction, after the solution is left to stand, centrifuge with a high-speed centrifuge for 10min at a speed of 8000rpm / min, then the precipitate is washed, Separate again until the supernatant becomes cloudy. The obtained cellulose nanocrystal suspension was ultrasonicated to obtain a stable cellulose nanocrystal suspension. The average size of the obtained cellulose crystal grains was measured to be about 160 nm, the yield was 77%, and the PDI was 1.5.

Embodiment 2

[0037] The types of raw materials used, the dosage and the process flow are the same as in Example 1, except that the soaking time of pulp cellulose in NaOH solution is extended to 72 hours to obtain a stable suspension of cellulose nanocrystals. The size is about 150 nm, the yield is 81%, and the PDI is 1.4.

Embodiment 3

[0039] After soaking 5g of α-cellulose with 250ml, 4wt% NaOH solution for 48 hours, filter and wash with deionized water until neutral, take this alkali-pretreated cellulose, add 0.078 gram of CuSO 4 ·5H 2 O, add 100 ml of 64wt% sulfuric acid, stir at 50°C for 1.5h, add deionized water to terminate the reaction, after the solution is allowed to stand, centrifuge at a speed of 8000rpm / min for 10min with a high-speed centrifuge, and then wash the precipitate , and separated again until the supernatant became cloudy. The obtained cellulose nanocrystal suspension was ultrasonicated to obtain a stable cellulose nanocrystal suspension with an average particle size of about 200 nm, a yield of 83%, and a PDI of 1.5.

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Abstract

The invention provides an efficient and quick cellulose nanocrystalline preparing method.According to the method, a cellulose raw material is pretreated with aqueous alkali and then subjected to acidolysis, and inorganic salt containing metal ions is added during acidolysis to serve as a promoter to promote acidolysis reaction.Reaction condition is mild and easy to control, raw materials needed by reaction are simple and easy to obtain, and the method can be widely applied to preparation of cellulose nanocrystalline from various cellulose raw materials.

Description

【Technical field】 [0001] The invention belongs to the field of nanomaterial preparation and also belongs to the field of macromolecules, in particular to a method for preparing cellulose nanocrystals. 【Background technique】 [0002] Natural cellulose is the most abundant biomass material in nature, and its annual output can reach 1.5×10 12 Ton. Cellulose nanocrystals with nanometer size can be obtained by extracting the crystalline regions of cellulose. Cellulose nanocrystals have many excellent properties, such as it has a large aspect ratio, and the length varies from hundreds of nanometers to several microns; it has high mechanical strength, and its Young's modulus is similar to that of aramid fibers It is higher than steel, and its tensile strength is similar to that of aluminum; cellulose nanocrystals have good thermal stability, and the thermal expansion coefficient is generally below 0.1ppm / K, which is comparable to carbon fiber. Cellulose nanocrystals can be orien...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/02D21C9/00D21C9/02
CPCC08B15/02D21C9/004D21C9/02
Inventor 周丽娟张建明段咏欣
Owner QINGDAO UNIV OF SCI & TECH
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