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Green method of functionally modified nano-crystalline cellulose

A nanocellulose, functionalized technology, applied in fermentation and other directions, can solve the problems of harsh reaction conditions, high process requirements, complex reaction routes, etc., and achieve the effects of mild reaction conditions, high catalytic efficiency, and simple process routes.

Inactive Publication Date: 2016-11-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all have defects and deficiencies to a certain extent, strict requirements on equipment, high process requirements, and easy damage to fibers, and most of these modification methods must be carried out in toxic organic solvents such as toluene and tetrahydrofuran. , the reaction conditions are harsh, the reaction route is complex, and the cost of industrial implementation is high

Method used

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  • Green method of functionally modified nano-crystalline cellulose
  • Green method of functionally modified nano-crystalline cellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1: Dry 0.5 g of microcrystalline cellulose at 50°C for 48 hours;

[0035] Step 2: Use [BMIM]HSO 4 Prepare the cellulose obtained in the first step into a mixture with a cellulose mass percentage concentration of 5%, and stir at a constant temperature of 70°C for 1 hour;

[0036] The third step: the solution obtained in the second step is lowered to room temperature, and lipase CRL and ionic liquid [BMIM]BF are added 4 ([BMIM]HSO 4 / [BMIM]BF 4 The mass ratio is 3:5) and methyl laurate, the amount of lipase CRL is 20% of the mass of microcrystalline cellulose, the molar ratio of methyl laurate to microcrystalline cellulose is 3:1, and react at 50°C for 3h; ;

[0037] Step 4: Cool the solution obtained in Step 3 to room temperature, add absolute ethanol to wash, centrifuge, remove the supernatant, and dry the obtained precipitate at 60° C. for 24 hours to obtain functionalized modified nanocellulose. The degree of substitution of the functionalized modified nanoc...

Embodiment 2

[0044] Step 1: Dry 0.5 g of microcrystalline cellulose at 50°C for 48 hours;

[0045] Step 2: Use [EMIM]HSO 4 Prepare the cellulose obtained in the first step into a mixture with a cellulose mass percentage concentration of 5%, and stir at a constant temperature of 100°C for 2 hours;

[0046] The third step: the solution obtained in the second step is lowered to room temperature, and lipase CRL and ionic liquid [BMIM]BF are added 4 ([BMIM]HSO 4 / [BMIM]BF 4 The mass ratio is 3:5) and methyl laurate, the amount of lipase CRL is 15% of the mass of microcrystalline cellulose, the molar ratio of methyl laurate to microcrystalline cellulose is 3:1, and react at 60°C for 3h; ;

[0047] Step 4: Cool the solution obtained in Step 3 to room temperature, add absolute ethanol to wash, centrifuge, remove the supernatant, and dry the obtained precipitate at 60° C. for 24 hours to obtain functionalized modified nanocellulose. As detected by acid-base titration, the degree of substitutio...

Embodiment 3

[0050] Step 1: Dry 0.5 g of microcrystalline cellulose at 80°C for 48 hours;

[0051] Step 2: Use [BMIM]HSO 4 Prepare the cellulose obtained in the first step into a mixture with a cellulose mass percentage concentration of 10%, and stir at a constant temperature of 80° C. for 3 hours;

[0052] The third step: the solution obtained in the second step is lowered to room temperature, and lipase CRL and ionic liquid [BMIM]BF are added 4 ([BMIM]HSO 4 / [BMIM]BF 4 The mass ratio is 3:5) and methyl laurate, the amount of lipase CRL is 15% of the mass of microcrystalline cellulose, the molar ratio of methyl laurate to microcrystalline cellulose is 13:1, and react at 60°C for 5h; ;

[0053] Step 4: Cool the solution obtained in Step 3 to room temperature, add absolute ethanol to wash, centrifuge, remove the supernatant, and dry the obtained precipitate at 60° C. for 24 hours to obtain functionalized modified nanocellulose. The degree of substitution of the functionalized modified ...

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Abstract

The invention discloses a green method of functionally modified nano-crystalline cellulose. The method comprises the steps of adding dried cellulose raw materials into ionic liquid; heating and stirring at a constant temperature; cooling an obtained solution to room temperature; adding lipase, fatty acid methyl ester and ionic liquid, wherein the dosage of the lipase is 2 to 50 percent of the mass of the cellulose, and a mole ratio of the fatty acid methyl ester to the cellulose is 1:1 to 13:1; reacting for 1 to 8h at the temperature of 20 to 80 DEG C; after the reaction is finished and the solution is cooled, adding absolute ethyl alcohol for washing and centrifuging; removing supernate; drying an obtained precipitate for 12 to 48h at the temperature of 40 to 80 DEG C, thus obtaining the functionally modified nano-crystalline cellulose provided by the invention. The functionally modified nano-crystalline cellulose provided by the invention has the advantages of simplicity, high efficiency, good repeatability, green and environmental protection in technological process and a used reagent, and the like, and has wide application value in the fields such as membrane materials, drug-releasing materials and optical materials.

Description

technical field [0001] The invention relates to the field of production methods of nanocellulose, in particular to a green method for functionally modifying nanocellulose. Background technique [0002] Nanocellulose is a refined cellulose obtained by softening, activating, and enzymatically cutting natural cellulose molecules. Because of its high crystallinity, high transparency, high Young's modulus, and regeneration, it is currently used in high-performance The field of composite materials shows great application prospects. However, the specific surface area of ​​nanocellulose is large, and the surface contains a large number of hydroxyl groups. The cellulose particles are easily aggregated through the interaction of hydrogen bonds, and the agglomerated cellulose particles are difficult to disperse by physical methods. Therefore, preparing functionally modified nanocellulose, reducing the hydrophilicity and polarity of nanocellulose, and improving its interfacial compatib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P19/04
CPCC12P19/04
Inventor 赵光磊王凤丽稂雄妃李晓凤
Owner SOUTH CHINA UNIV OF TECH
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