Preparation process of nanocrystal cellulose

A nanocrystal and preparation technology, applied in the field of cellulose materials, can solve the problems of low purity, wide particle size distribution, and low yield of nanocrystalline cellulose, and achieve good particle size uniformity, simple preparation process, and high yield. Effect

Active Publication Date: 2017-06-09
SHENZHEN YOUPUHUI PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the length distribution of absorbent cotton is very wide (ranging from a few microns to several millimeters), the direct use of sulfuric acid hydrolysis results in insufficient destruction of the amorphous and subcrystalline regions of some fibers, while the crystalline regions of some fibers are excessively destroyed into single-molecule glucose. The resulting nanocrystalline cellulose has low purity, low yield and wide particle size distribution

Method used

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  • Preparation process of nanocrystal cellulose
  • Preparation process of nanocrystal cellulose
  • Preparation process of nanocrystal cellulose

Examples

Experimental program
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Embodiment 1

[0034] Commercially available pulp (α-cellulose-rich pulp made of cellulose) was added to a slicer and cut into 2 cm x 2 cm squares. Add 100g of cellulose slurry to 900ml of 1.0mol / L hydrochloric acid solution, carry out the first gradient hydrolysis reaction at 100°C, stir with an overhead stirrer at 300 rpm for 20 minutes, filter and wash with water, and obtain a solid content of 40wt%. Cellulose filter cake, the degree of polymerization is 320; add 1000ml of 45wt% sulfuric acid solution to the filter cake, carry out the second gradient hydrolysis reaction at 50°C, the reaction time is 30 minutes, filter and wash with water, and spray dry to obtain nanocrystalline cellulose. The physical characterization parameters are shown in Table 1, figure 1 , image 3 shown.

Embodiment 2

[0036] Commercially available pulp (α-cellulose-rich pulp made of cellulose) was added to a slicer and cut into 2 cm x 2 cm squares. Add 100g of cellulose slurry to 800ml of 3.0mol / L hydrochloric acid solution, carry out the first gradient hydrolysis reaction at 100°C, stir with an overhead stirrer at 300 rpm for 20 minutes, filter and wash with water, and obtain a solid content of 40wt%. Cellulose filter cake, the degree of polymerization is 300; add 1000ml of 30wt% sulfuric acid solution to the filter cake, carry out the second gradient hydrolysis reaction at 80°C, the reaction time is 30 minutes, filter and wash with water, and spray dry to obtain nanocrystalline cellulose. The physical characterization parameters are listed in Table 1.

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Abstract

The invention discloses a preparation process of nanocrystal cellulose and relates to the field of cellulose materials. The preparation process includes: adding mechanically-processed cellulose wood pulp into a hydrochloric acid solution to perform first-gradient hydrolysis reaction until polymerization degree is smaller than 350, filtering and cleaning, and draining; adding filter cakle into a sulfuric acid solution to perform second-gradient hydrolysis reaction until polymerization degree is smaller than 100, filtering and cleaning, and drying to obtain the nanocrystal cellulose. The preparation process has the advantages that the cellulose wood pulp is used as the raw material, the low-concentration hydrochloric acid solution is used to perform the first-gradient hydrolysis reaction before sulfuric acid hydrolysis, then the sulfuric acid solution is used to perform second-gradient hydrolysis reaction, the prepared nanocrystal cellulose is small in particle size and concentrated in particle size distribution, and the purity and yield of the nanocrystal cellulose are increased greatly.

Description

technical field [0001] The invention relates to the field of cellulose materials, in particular to a preparation process of nanocrystalline cellulose. Background technique [0002] With the increasingly prominent problems of energy crisis and environmental pollution, environmentally friendly and renewable materials have been extensively studied. Cellulose is the most abundant natural degradable polymer on earth, and it is an environmentally friendly material with good biocompatibility. Nanocrystalline cellulose (NCC) is the smallest physical structural unit obtained after hydrolysis of cellulose, with a diameter of less than 100nm, a large aspect ratio, high specific surface area and high strength (its strength is 1 / 3 of that of carbon nanotubes. , is 8 times that of steel) low-density nanomaterials, which have broad application prospects. [0003] The production process of nanocrystalline cellulose usually includes acid hydrolysis, TEMPO oxidation and mechanical method. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 张海龙谭玉圆段民英
Owner SHENZHEN YOUPUHUI PHARM CO LTD
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