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Preparation method of nanocellulose film precipitated by applying water solution

A technology of nanocellulose and application of aqueous solution, applied in the field of preparation of cellulose, nanocellulose and nanocellulose film, can solve the problems of difficult recovery and processing reaction, low yield, and high requirements for reaction equipment

Active Publication Date: 2013-12-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current preparation methods of nanocellulose include: (1) Preparation of nanocellulose by acid method, that is, using inorganic acid or organic acid as a catalyst to provide high-concentration hydrogen ions into the amorphous region of cellulose to break hydrogen bonds and hydrolyze it to generate glucose At the same time, the cellulose chain is cracked to a certain extent, resulting in a decrease in the degree of cellulose polymerization, thereby obtaining nanocellulose. In 1947, Nickerson and Habrle used hydrochloric acid and sulfuric acid to hydrolyze wood and cotton wool to prepare nanocellulose colloidal dispersion. However, this method requires the use of strong acid, which requires high reaction equipment, and will produce acid waste liquid, which is difficult to recycle and process; (2) enzymatic hydrolysis to prepare nanocellulose, that is, using cellulase to selectively enzymatically decompose amorphous Cellulose leaves some cellulose crystals. This method can improve the quality and purity of nanocellulose without using chemicals, but has the defects of low yield and high cost; (3) TEMPO oxidation method to prepare nanocellulose, That is, TEMPO is used to catalyze oxidation to prepare nanocellulose. TEMPO acts as a catalyst to promote the selective oxidation of primary hydroxyl groups on cellulose C6 to oxidize it into polyglucuronic acid, which makes the surface of the filaments negatively charged. Electrostatic repulsion is generated to obtain a stable nanocellulose colloidal dispersion, and TEMPO is expensive in this method

Method used

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  • Preparation method of nanocellulose film precipitated by applying water solution
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  • Preparation method of nanocellulose film precipitated by applying water solution

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Weigh 1g of bamboo dissolving pulp dry pulp, and dissolve the bamboo dissolving pulp dry pulp in the mixed solution of 100ml sodium hydroxide, urea and water under the condition of -8°C, the content of sodium hydroxide, urea and water in the mixed solution is The mass ratio is 7:12:81. After stirring for 3 minutes under the condition of maintaining -8°C, centrifuge at a centrifugal speed of 10,000 r / min for 10 minutes to remove impurities, and obtain 100 ml of a clear and viscous cellulose solution. After naturally warming up to room temperature, 100ml of water was added dropwise to the 100ml cellulose solution while stirring, and the cellulose molecules were gradually precipitated to obtain a nanocellulose colloidal dispersion. Two PVDF filter membranes with a pore size of 0.22 μm (Polyvinylidene Fluoride GVWP14250, 0.22 μm pore size, Millipore, Ireland) were stacked, and the filter press (142-mm Millipore Hazardous Waste Filtration System, Millipore, Ireland) was used...

Embodiment 2

[0037] Weigh 1g of dry hardwood bleached pulp, and dissolve the dry hardwood bleached pulp in 100ml of a mixed solution of sodium hydroxide, urea and water at -8°C. In the mixed solution, sodium hydroxide, urea and The mass ratio of water is 5:15:80. After stirring for 3 minutes under the condition of maintaining -8°C, centrifuge at a centrifugal speed of 10,000 r / min for 10 minutes to remove impurities, and obtain 100 ml of a clear and viscous cellulose solution. After naturally warming up to room temperature, 150 ml of water was added dropwise to 100 ml of cellulose solution while stirring, and the cellulose molecules were gradually precipitated to obtain a nanocellulose colloidal dispersion. Two PVDF filter membranes with a pore size of 0.22 μm (Polyvinylidene Fluoride GVWP14250, 0.22 μm pore size, Millipore, Ireland) were stacked, and the filter press (142-mm Millipore Hazardous Waste Filtration System, Millipore, Ireland) was used to prepare The nanocellulose colloidal d...

Embodiment 3

[0039] Weigh 1g of microcrystalline cellulose, and dissolve the microcrystalline cellulose in a mixed solution of 100ml of sodium hydroxide, urea and water at -15°C, the mass ratio of sodium hydroxide, urea and water in the mixed solution is 10 :10:80. After stirring for 3 minutes under the condition of maintaining -15°C, centrifuge at a centrifugal speed of 10000r / min for 10 minutes to remove impurities, and obtain 100ml of clear viscous cellulose solution. After naturally warming up to room temperature, 200ml of water was added dropwise to 100ml of cellulose solution at room temperature while stirring, and the cellulose molecules were gradually precipitated to obtain nanocellulose colloidal dispersion. Two PVDF filter membranes with a pore size of 0.22 μm (Polyvinylidene Fluoride GVWP14250, 0.22 μm pore size, Millipore, Ireland) were stacked, and the filter press (142-mm Millipore Hazardous Waste Filtration System, Millipore, Ireland) was used to prepare The nanocellulose c...

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Abstract

The invention discloses a preparation method of a nanocellulose film precipitated by applying a water solution. The preparation method comprises the following steps: dissolving cellulose with concentration of 10-40g / L into a mixed solution of sodium hydroxide, urea and water at minus 15-minus 8 DEG C; after heating the cellulose solution to the room temperature, dropwise adding water to the cellulose solution to precipitate cellulose to obtain nanocellulose colloid dispersion liquid; filter-pressing the nanocellulose colloid dispersion liquid to obtain the nanocellulose film, wherein the mixed solution contains 5-10% of sodium hydroxide, 10-15% of urea and the balance of water by mass percent, and the volume ratio of water to the cellulose solution is (1-3):1. The method overcomes the defects of difficulty in acid waste liquor recovery, high preparation cost, high preparation energy consumption, heavy environmental pollution and the like in the existing preparation method of nanocellulose and the film thereof, and has the advantages of simplicity and high efficiency in operation, solvent reusability, environment friendliness and low energy consumption.

Description

technical field [0001] The invention relates to cellulose, in particular to a nano-cellulose, in particular to a method for preparing a nano-cellulose film precipitated by an aqueous solution, and belongs to the field of material processing. Background technique [0002] With the rapid development of human society and the irrational use of fossil energy, the problems of energy shortage and environmental pollution are becoming more and more serious, and people are paying more and more attention to the research of cellulose, an inexhaustible and renewable resource. Compared with ordinary cellulose, nanocellulose has broad application prospects in the fields of nano fine chemical industry, nano medicine, nano food, nano composite materials and new energy because of its particularity in aggregated structure and physical properties. [0003] The current preparation methods of nanocellulose include: (1) Preparation of nanocellulose by acid method, that is, using inorganic acid or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J3/05C08L1/02
Inventor 邱学青林吼坑楼宏铭杨东杰
Owner SOUTH CHINA UNIV OF TECH
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