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Method for preparing cellulose nano-fibril film by utilizing wood powder

A technology of nanofibrils and lignocellulose, which is applied in the field of preparation of lignocellulose nanofibrils, can solve the problems of low hydrolysis yield and achieve the effect of simple and easy grinding treatment

Inactive Publication Date: 2013-01-30
襄垣县鑫瑞达连氏塑木制造有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the perspective of cost and equipment, biological pretreatment shows unique advantages. Specific lignin enzymes can be used to treat raw materials to decompose lignin and improve lignin digestibility, but the hydrolysis rate after biological pretreatment is very low

Method used

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  • Method for preparing cellulose nano-fibril film by utilizing wood powder

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Experimental program
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Effect test

Embodiment 1

[0008] 1. Chemical pretreatment,

[0009] 1) Screen 60-70 mesh dry wood powder, accurately weigh 4g, add 300ml of toluene and ethanol mixture, the volume ratio is 2:1, into the Soxhlet extractor, extract at 90°C for 7h, remove For extracts such as ash, dry the extracted wood powder at room temperature for 24 hours to volatilize the toluene and ethanol on the surface;

[0010] 2) Transfer the dried wood powder into a 250ml beaker, add 150ml of distilled water, 1ml of glacial acetic acid and 1.5g of sodium chlorite, stir well with a glass rod, seal the mouth of the cup with plastic wrap, and put it in a constant temperature water bath at 75°C Heat for 1 hour; put a magnet in the cup for constant stirring to make the reaction more complete; add 1ml of glacial acetic acid and 1.5g of sodium chlorite to the beaker after 1 hour, and continue heating in a water bath at 75°C for 1 hour, repeating this 6 times , until the sample turns white; then filter with a vacuum filter pump and a...

Embodiment 2

[0025] Different cellulose nanofibers are prepared from poplar wood fibers: the chemical treatment steps are the same as above. After the chemical treatment is completed, the cellulose fibers are prepared with distilled water into an aqueous suspension with a mass fraction of cellulose fibers of 0.4%, a total of 500 ml, which are divided into five equal parts after thorough stirring, that is, the volume of each part is 100 ml. Then pour 300 ml of distilled water into each part of the cellulose fiber aqueous suspension, and stir thoroughly, so as to obtain five parts of the cellulose fiber water suspension with a mass fraction of 0.1%, each with a volume of 400 ml. Finally, the five aqueous cellulose fiber suspensions were ground for 1, 3, 7, 15 and 30 times respectively, and the rotation speed of the grinding disc was 1500 rpm. Thus, five cellulose nanofibers with different sizes were prepared, named CNF 1, CNF 3, CNF 7, CNF 15 and CNF 30, respectively.

Embodiment 3

[0027] Ultrasonic treatment and high-pressure homogenization of nanocellulose fibrils / plexiglass (CNF / PMMA) nanocomposites: re-preparation of cellulose nanofibers from poplar wood fibers,

[0028] The specific operation is as follows: after the chemical treatment, it is also configured into three water suspensions with a mass fraction of cellulose fibers of 0.1%, and then two of them are subjected to 7 grinding treatments, and then ultrasonic grinding is performed on the basis of 7 grindings. Treatment and high-pressure homogenization, the ultrasonic power is 1000 W, the time is 60 min, and the pressure of high-pressure homogenization is 1000 bar, and the time is 90 min. In this way, different cellulose nanofibers are prepared, and then a suction filtration operation is performed to prepare a cellulose nanofiber film, and then a corresponding nanocomposite film is prepared by an impregnation method.

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Abstract

The invention relates to a method for preparing a cellulose nano-fibril film by utilizing wood powder, which comprises the following steps: 1) chemically pre-processing; 2) mechanically separating; and 3) preparing a film. The method has the advantages: the acid-base pre-processing is combined with wood powder grinding and is adopted for preparing; the lignin in the wood powder is removed by mainly utilizing sodium chlorite under an acidic condition; the half-fibril is removed by using the diluted potassium hydroxide and the remained substrate is cellulose; and the diluted hydrochloric acid is used for splitting the cellulose. The acting force of hydrogen bonds in the fibril is reduced by adopting the splitting treatment, so that the biomass cellulose nano-fibril at high length-diameter ratio is obtained; the mineral substance in the fiber is removed by utilizing HCl treatment, the alkali insoluble half-cellulose in the purified cellulose is influenced and the effect of purifying the cellulose fiber is achieved; the chemical constituents are detected through Fourier transform infrared; the grinding treatment is simple and easy to operate and the mass production is performed; the modulus of elasticity is 3105.27MPa; and the tensile strength is 64.24MPa.

Description

technical field [0001] The invention relates to a method for preparing lignocellulose nanofibrils. The invention belongs to the technical field of biomass nanofibers. Background technique [0002] The separation process of biomass cellulose nanofibrils mainly includes pretreatment and mechanical separation. Two main treatment methods are used throughout the separation process: mechanical treatment and chemical treatment. Although the mechanical treatment consumes a certain amount of energy, the raw materials can be fully utilized; in the chemical treatment, only about half of the raw materials are used, and the other half of the raw materials are removed, but the stirring in the experiment will promote the generation of chemical heat and effectively remove impurities. The heat of combustion is the energy consumed during the entire chemical process. Currently, there is a method of oxidation pretreatment, that is, using TEMPO as a medium to catalyze oxidation to prepare cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21B1/12
Inventor 李爱军李大纲顾文彪薛莹莹胡月潘佳陈振东李明珠李雪婷
Owner 襄垣县鑫瑞达连氏塑木制造有限公司
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