Preparation method of narrow-distribution cellulose nanocrystalline

A cellulose and nanocrystal technology, applied in nanotechnology and other directions, can solve the problems of wide and uneven particle distribution, and achieve the effects of simple removal, low cost and wide application prospects.

Inactive Publication Date: 2012-08-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method of narrowly distributed cellulose nanocrystals. The preparation process of the method is simple and easy to operate, and the chemicals used are volatile acids and alkalis, which are low in cost and easy to remove; The environment is non-polluting and suitable for industrial scale production; the prepared cellulose nanocrystals have the advantages of small size and narrow distribution, easy size adjustment, large specific surface area, and high reactivity, effectively avoiding wide distribution of cellulose nanocrystal particles, Inhomogeneity and other problems, has a wide range of application prospects

Method used

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  • Preparation method of narrow-distribution cellulose nanocrystalline

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Experimental program
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Effect test

Embodiment 1

[0018] Commercially available microcrystalline cellulose was fully soaked in a hydrochloric acid solution with a concentration of 5 mol / L, and then transferred to a hydrothermal kettle lined with polytetrafluoroethylene, in which the solid content of microcrystalline cellulose was 0.008 g / mL. The reaction was carried out at 110° C. for 3 hours. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. After static layering, the supernatant was removed, and repeated several times until the dispersion formed a stable suspension. Add 2mol / L ammonia solution to adjust the pH of the solution to 7. The volatile components are removed by heating to obtain a uniformly distributed cellulose nanocrystal dispersion. The particle size distribution of rod-shaped or elliptical cellulose nanocrystals is 20-30nm as measured by the nanometer particle size and potential analyzer. By freeze-drying the cellulose nanocrystal dispers...

Embodiment 2

[0020] Commercially available microcrystalline cellulose was fully soaked in a hydrochloric acid solution with a concentration of 6 mol / L, and then transferred to a hydrothermal kettle lined with polytetrafluoroethylene, in which the solid content of microcrystalline cellulose was 0.0125 g / mL. The reaction was carried out at 100° C. for 4 hours. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. After static layering, the supernatant was removed, and repeated several times until the dispersion formed a stable suspension. Add 1 mol / L ammonia solution to adjust the pH of the solution to 7. After heating to remove volatile components, a uniformly distributed cellulose nanocrystal dispersion liquid is obtained; the diameter distribution of rod-shaped or elliptical cellulose nanocrystals is 28-42 nm as measured by a nanometer particle size and potential analyzer. By freeze-drying the cellulose nanocrystal dispe...

Embodiment 3

[0022] Commercially available microcrystalline cellulose was fully soaked in 3 mol / L acetic acid solution, and then transferred to a polytetrafluoroethylene-lined hydrothermal kettle, in which the solid content of microcrystalline cellulose was 0.006 g / mL. The reaction was carried out at 120° C. for 5 hours. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. After static layering, the supernatant was removed, and repeated several times until the dispersion formed a stable suspension. Add 1 mol / L ammonia solution to adjust the pH of the solution to 7. After heating to remove volatile components, a uniformly distributed cellulose nanocrystal dispersion liquid is obtained; the diameter distribution of rod-shaped or elliptical cellulose nanocrystals is 35-50 nm as measured by a nanometer particle size and potential analyzer. By freeze-drying the cellulose nanocrystal dispersion, cellulose nanocrystals with hig...

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Abstract

The invention relates to a preparation method of narrow-distribution cellulose nanocrystalline, comprising the following steps of: (1) placing microcrystalline cellulose into volatile acid liquor, transferring to a hydrothermal kettle and reacting for 1-5h at 100-120 DEG C; (2) after naturally cooling the hydrothermal kettle, diluting a reaction product by using deionized water, removing supernatant liquor after standing for layering, adding a volatile alkali solution, regulating the pH value of the solution to 7, and then heating to obtain cellulose nanocrystalline dispersion liquor; and drying the dispersion liquor to obtain the cellulose nanocrystalline. The preparation method has the advantages of simple process, easiness for operation and no environmental pollution in the whole preparation process and is suitable for industrial scale production; and the prepared cellulose nanocrystalline has the advantages of small size, narrow distribution, easiness for controlling the size, large specific surface area and high reactivity and effectively avoids the problems of wide distribution, nonuniformity and the like of the particles of the cellulose nanocrystalline, thereby having wideapplication prospect.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose nanocrystals, in particular to a preparation method of narrowly distributed cellulose nanocrystals. Background technique [0002] Cellulose is an inexhaustible and inexhaustible renewable natural polymer synthesized mainly by plants through photosynthesis in nature. The cellulose microcrystal processed from natural cellulose has been widely used in food, medicine, cosmetics and paint stabilizer (as CN101481424A; CN1448427A; CN1340651A), plastics and rubber filler (as CN1369508A; CN1340651A) and In the production of synthetic leather (such as CN101070352A; CN1220271A). The sizes of cellulose microcrystals are different, and their uses are also different. For example, nanocrystals with a size of 2 to 15 μm can be used as fat substitutes or dietary fibers; nanocrystals with a size of 2 to 200 μm can be used as fillers, adhesives in the pharmaceutical industry. agent, adsorbent and anti-cakin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/08B82Y40/00
Inventor 秦宗益余厚咏周哲徐晓军肖婉瑶程淼
Owner DONGHUA UNIV
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