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Nanometer microcrystalline cellulose preparation method

A technology of microcrystalline cellulose and nanocrystalline, which is applied in the fields of biochemical engineering and chemical engineering, can solve problems such as low efficiency, environmental pollution, and low production rate, and achieve simple and easy preparation process, reduce production cost, and improve utilization rate Effect

Active Publication Date: 2014-04-30
JIANGSU UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the nano-microcrystalline cellulose suspension prepared by sulfuric acid hydrolysis has high stability, a large amount of high-concentration sulfuric acid and relatively high-concentration hydrochloric acid are required in the preparation process, so it is easy to cause corrosion of equipment and environmental pollution. Therefore, sulfuric acid method Hydrolysis is still limited to the laboratory research stage so far, and cannot enter the industrialization stage of mass production
At the same time, the high-pressure mechanical dissociation method has begun to enter the stage of medium-scale mass production, but the problem of excessive power consumption has not yet been resolved
If nanocellulose is extracted from wood, it also faces the same environmental pollution problems as the paper industry; when extracting nanocellulose from bacterial cellulose, it faces the problems of low yield and low production rate; extracting nanocellulose from tunicate cellulose When extracting cellulose, it also faces the problem of low yield; when extracting from some agricultural by-products with low cellulose content, it faces the problem of low efficiency and low performance of the final product

Method used

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  • Nanometer microcrystalline cellulose preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Example 1: First, take 1 g of microcrystalline cellulose and add 100 g of an aqueous solution with a mass fraction of 10% N-methylmorpholine-N-oxide, and heat and stir at 50°C for 20 minutes to fully swell the fibers of the microcrystalline cellulose , to obtain a mixed solution; secondly, after treating the mixed solution with a 60w ultrasonic wave for 30 minutes, add 10 g of hydrogen phosphate ionic liquid, stir evenly, and then use a 60w ultrasonic wave for 30 minutes; then, add water and stir evenly, and the amount of water added is N-methyl? 0.5 times the volume of the morphine-N-oxide solution, the mixed solution naturally settles and is divided into upper and lower layers, collects the lower layer, removes impurities, and freeze-dries to obtain nano-microcrystalline cellulose; finally, the treatment agent is recovered, and the supernatant is taken, Centrifuge at 10000r / min for 5min, distill under reduced pressure at 80°C for 30min to remove water and low-boiling i...

Embodiment 2

[0021] Example 2: First, take 1 g of microcrystalline cellulose and add 200 g of an aqueous solution with a mass fraction of 50% N-methylmorpholine-N-oxide, and heat and stir at 70°C for 5 minutes to fully swell the fibers of the microcrystalline cellulose , to obtain a mixed solution; secondly, after treating the mixed solution with an 80w ultrasonic wave for 25min, add 5g of bisulfate ionic liquid, stir evenly, and then use an 80w ultrasonic wave for 25min; The volume of -N-oxide solution is equal, the mixed solution naturally settles and is divided into upper and lower layers, the lower layer is collected, impurities are removed, and nano-microcrystalline cellulose is obtained by freeze-drying; finally, the treatment agent is recovered, and the supernatant is taken, 10000r / min Centrifuge for 5 minutes, distill under reduced pressure at 90°C for 30 minutes; heat and distill under reduced pressure at 150°C for 30 minutes to remove water, and sublimate N-methylmorpholine-N-oxid...

Embodiment 3

[0023] First, take 1 g of microcrystalline cellulose and add it to 100 g of an aqueous solution with a mass fraction of 80% N-methylmorpholine-N-oxide, and heat and stir at 60°C for 10 minutes to fully swell the fibers of microcrystalline cellulose to obtain a mixed solution ; Secondly, after treating the mixed solution with a 90w ultrasonic wave for 20 minutes, add 8g of hydrogen phosphate ionic liquid, stir evenly, and then use a 90w ultrasonic wave for 20min; then, add water and stir evenly, and the amount of water added is N-methylmorpholine-N- 0.6 times the volume of the oxide solution, the mixed solution naturally settles and is divided into upper and lower layers, collects the lower layer, removes impurities, freeze-dries to obtain nano-microcrystalline cellulose; finally, recovers the treatment agent, takes the supernatant, and centrifuges at 10,000r / min 5min, vacuum distillation at 85°C for 30min, heating and vacuum distillation at 145°C for 30min to remove water, and ...

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Abstract

The present invention discloses a nanometer microcrystalline cellulose preparation method, which comprises: (1) adopting N-methylmorpholine-N-oxide and an ion liquid to treat microcrystalline cellulose; and (2) recovering the treatment agent. According to the present invention, the nanometer microcrystalline cellulose preparation method has the following advantages that: microcrystalline cellulose is adopted as a raw material, and can be extracted from plants, such that the source is wide, and the natural plant fiber utilization rate is substantially increased; the N-methylmorpholine-N-oxide and the ion liquid are subjected to coupling use, and the treatment is performed to obtain the fragmented nanometer microcrystalline cellulose; the N-methylmorpholine-N-oxide and the ion liquid can be recycled after being treated so as to reduce the nanometer microcrystalline cellulose production cost; and the nanometer microcrystalline cellulose preparation process has characteristics of simpleness, easy performing and green environmental protection, and no corrosion on equipment, environmental pollution and other problems exists.

Description

technical field [0001] The invention relates to a method for preparing cellulose, in particular to a method for preparing nano-microcrystalline cellulose, which belongs to the fields of biochemical engineering and chemical engineering. Background technique [0002] Cellulose is the most widely distributed and most abundant polysaccharide in nature. It has the advantages of degradability, regeneration, low density and no pollution to the ecological environment. The cellulose synthesized by photosynthesis in the world can reach hundreds of billions of tons every year. Therefore, cellulose has become an environment-friendly and per capita non-petroleum comparable green environmental protection resource. However, natural cellulose has some defects in both physical form and chemical properties, such as poor thermal solubility, chemical corrosion resistance, and limited strength. Nanocrystalline cellulose (Nanocrystalline Cellulose, NCC) refers to cellulose with at least one dime...

Claims

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Application Information

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IPC IPC(8): C08B15/02C08B15/00
Inventor 李强徐术娟季更生屠洁孟春凤
Owner JIANGSU UNIV OF SCI & TECH
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