Preparation method of bamboo holocellulose nanofiber with high length-diameter ratio and high hemicellulose content

A technology of hemicellulose and nanofibers, applied in the direction of cellulose/protein conjugated artificial filaments, nanotechnology, fiber chemical characteristics, etc. low, can not fully meet the needs of use, etc., to achieve the effect of environmental friendliness, short time and easy operation

Active Publication Date: 2021-11-09

NANJING FORESTRY UNIV

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Problems solved by technology

[0004] CN110128555A discloses a method of obtaining cellulose nanocrystals by treating pretreated biomass as raw material with organic solvents, ionic liquids and cellulose solvents, However, it takes a long time to process and uses more organic solvents, and the highest yield of cellulose nanocrystals i...

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Abstract

The invention discloses a preparation method of bamboo holocellulose nanofiber with high length-diameter ratio and high hemicellulose content. The method comprises the following steps of treating bamboo holocellulose by adopting an acetic acid-assisted eutectic solvent under the condition of microwave radiation, performing solid-liquid separation after the treatment is finished, dispersing the solid, performing homogenizing, and preparing the bamboo holocellulose nanofiber through a micro-jet machine, wherein the length-diameter ratio of the bamboo holocellulose nanofiber is not less than 300, and the hemicellulose content is not less than 14%. According to the method, the length-diameter ratio of nano holocellulose (HCNF) can be effectively increased, and the hemicellulose content of the obtained HCNF and the acetylation degree of cellulose are relatively high; and the obtained bamboo nano holocellulose has the advantages of being adjustable in size, uniform in dispersion and the like. Meanwhile, the method also has the advantages of simple process, mild reaction conditions, environmental friendliness, easiness in operation and the like, and has relatively high application potential.

Application Domain

Conjugated cellulose/protein artificial filamentsNanotechnology

Technology Topic

Polymer chemistryNanofiber +3

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Examples

Experimental program(4)

Example Embodiment

[0032] Example 1

[0033] Preparation method of bamboo cellulose nanofibers of high long diameter ratio high tanks, steps are as follows:

[0034] (1) Preparation of low-molten solvent (DES): zinc acetate (ZA) as a hydrogen bond donor, choline choline (CHCl) as hydrogen bond receptor, uniform mixing with receptor molar ratio 1: 2 The mixture was stirred at 80 ° C for 4 h by magnetic force until a uniform transparent liquid appeared.

[0035] (2) Preprocessing: 0.5 g of bamboo cellulose powder and 25 ml of zinc chloride (ZAC) to the TEFLON container of the microwave reactor. The solid solution of the cellulose powder and the DES of the bamboo tape is 1:50 (g / ml), and acetic acid, the molar ratio of acetic acid and DES is 1: 1 (ZAC1-1), or 1: 2 (ZAC2-1) , Or 1: 3 (zac3-1). The mixture is mixed using a glass rod. The mixture was treated at 120 ° C, the microwave irradiation power was 600 W for 10 minutes. After preprocessing, the mixture was cooled to room temperature, and the powder residue was freeze dry after washing.

[0036](3) Preparation of HCNF: The decreasing of bamboo cellulose after pre-treatment was re-dispersed in deionized water, and sample homogenesis was 15 min with a homogenizer. Then quickly centrifuge, the supernatant passes through the microjet, and the operating pressure is 600 bar, and the operation is carried out 5 times to obtain HCNF.

Example Embodiment

[0037] Example 2

[0038] Preparation method of bamboo cellulose nanofibers of high long diameter ratio high tanks, steps are as follows:

[0039] (1) Preparation of low-molten solvent (DES): zinc acetate (ZA) as a hydrogen bond donor, choline choline (CHCl) as hydrogen bond receptor, uniform mixing with receptor molar ratio 1: 2 The mixture was stirred at 80 ° C for 4 h by magnetic force until a uniform transparent liquid appeared.

[0040] (2) Preprocessing: 0.5 g of bamboo cellulose powder and 25 ml of zinc chloride (ZAC) to the TEFLON container of the microwave reactor. The solid-liquid ratio of the bamboo cellulose powder and DES is 1: 50 (g / ml), and acetic acid, the molar ratio of acetic acid and DES is 1: 1 (ZAC1-2), or 1: 2 (ZAC2-2) , Or 1: 3 (ZAC3-2). The mixture is mixed using a glass rod. The mixture was taken at 140 ° C and the microwave irradiation power was taken at 600 W. After preprocessing, the mixture was cooled to room temperature, and the powder residue was freeze dry after washing.

[0041] (3) Preparation of HCNF: The decreasing of bamboo cellulose after pre-treatment was re-dispersed in deionized water, and sample homogenesis was 15 min with a homogenizer. Then quickly centrifuge, the supernatant passes through the microjet, and the operating pressure is 600 bar, and the operation is 5 times to obtain HCNF.

Example Embodiment

[0042] Example 3

[0043] The results obtained by the preparation of Examples 1, 2 were named ZAC1-1, ZAC2-1, (ZAC3-1, ZAC1-2, ZAC2-2, ZAC3-2, ZAC3-2, were characterized, and the results were shown in Table 1 Shows. The specific method is as follows:

[0044] 1) The calculation formula of the recovery rate is: recovery = HcNF mass (G) / bamboo cellulose powder mass (g) * 100%.

[0045] 2) AFM observation: Dilute the nano-stricken cellulose suspension 0.5%, dried on a smooth cloud master, after natural air dried, using an atomic force microscope to observe nanofiber morphology, obtain average length (nm), average width (nm) and long Ratio.

[0046] 3) Determination of crystallinity: The instrument used is an X-ray diffraction instrument, crystallinity (%) = crystalline zone peak area / (crystalline zone peak area + amorphous zone peak area) * 100%.

[0047] 4) Determination of glucan and xylan content: Using US energy laboratory special wood fiber component assay, after hydrolysis of sulfuric acid, the ion chromatography is used to measure the content content in hydrolyzing liquid;

[0048] Glucose content (%) = glycoose content (g) / original enzyme mass (G) * 100%;

[0049] Wooden glycan content (%) = hydrolyzate content (g) / original enzyme resistance mass (g) * 100%;

[0050] 5) Determination of acetylation: assays the lyophilized sample peak fitting by X-ray photoelectron spectrometer, acetylated = 288.5 eV peak area / (284.7 eV peak area + 286 eV peak area).

[0051] Table 1 Recycling rate and component analysis data of nano-stroke cellulose

[0052]

[0053]

[0054] figure 1 It is a transmissive electron microscope (TEM) diagram of nano-integrated cellulose after low-molten solvent pretreatment;

[0055] figure 2 It is a particle size distribution of nano-integrated cellulose after low-molten solvent pretreatment; figure 1 , figure 2 And the results of Table 1 are known that nano-integrated cellulose has typical fiber morphology, uniform dispersion, high and scales can be regulated; various embodiments have reasonable distribution of nanomic fibrin scale, obtained HCNF hemicellulose content and The degree of acetylation of cellulose is higher.

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

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Classification and recommendation of technical efficacy words

High aspect ratio
Simple process

Preparation method of bamboo holocellulose nanofiber with high length-diameter ratio and high hemicellulose content

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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