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Method for preparing nanocellulose microfibrils through pretreatment of ternary eutectic solvent

A low eutectic solvent and nanocellulose technology, which is applied in fiber raw material processing, textile and papermaking, etc., can solve problems such as poor effect, and achieve the effects of simple operation, shortened pretreatment time, and small particle size.

Active Publication Date: 2021-05-28
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The deep eutectic solvents currently used in the pretreatment of lignocellulose are binary solvent systems composed of a hydrogen bond acceptor and a hydrogen bond donor, but the effect is not good; and currently for the use of multiple deep eutectic solvents There are few reports on the pretreatment of lignocellulosic biomass and the separation and preparation of nanocellulose. Therefore, the study of ternary deep eutectic solvents has broad application prospects for the pretreatment of lignocellulose and the preparation of cellulose nanofibers.

Method used

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  • Method for preparing nanocellulose microfibrils through pretreatment of ternary eutectic solvent
  • Method for preparing nanocellulose microfibrils through pretreatment of ternary eutectic solvent
  • Method for preparing nanocellulose microfibrils through pretreatment of ternary eutectic solvent

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Effect test

Embodiment 1

[0041] (1) Synthesis of ternary deep eutectic solvent: Weigh 28g choline chloride, 36g oxalic acid, 9.64g aluminum trichloride, mix the three and stir at 70°C until a uniform transparent liquid is formed to obtain Ternary deep eutectic solvent;

[0042](2) Pretreatment: Add 0.5g bagasse to the microwave digestion tank, then add 5g ternary deep eutectic solvent, and react at 80°C for 20min; for the accuracy of the experimental data, three parallel experiments were performed for each group of experiments; After completion, immediately put into an ice-water bath to stop the reaction, separate the solid from the liquid, dilute the liquid part by 20 times with distilled water, let it stand, and analyze and measure the sugar content in the reaction solution by HPLC. The solid part was washed with acetone aqueous solution (volume ratio of acetone and water 50:50, v / v) until the filtrate was colorless, and finally the solid part was freeze-dried to obtain pretreated bagasse. The cont...

Embodiment 2

[0045] (1) Synthesis of ternary deep eutectic solvent: take by weighing 28g choline chloride, 36g lactic acid, 9.64g aluminum trichloride, mix the three and stir at 70°C until a uniform transparent liquid is formed to obtain Ternary deep eutectic solvent;

[0046] (2) Pretreatment: Add 0.5g bagasse to the microwave digestion tank, then add 5g ternary deep eutectic solvent, and react at 100°C for 20min; for the accuracy of the experimental data, each group of experiments is done in three parallels; After completion, immediately put into an ice-water bath to stop the reaction, separate the solid from the liquid, dilute the liquid part by 20 times with distilled water, let it stand, and analyze and measure the sugar content in the reaction solution by HPLC. The solid part was washed with acetone aqueous solution (volume ratio of acetone and water 50:50, v / v) until the filtrate was colorless, and finally the solid part was freeze-dried to obtain pretreated bagasse. The contents o...

Embodiment 3

[0049] (1) Synthesis of ternary deep eutectic solvent: Weigh 28g choline chloride, 36g oxalic acid, 9.64g aluminum trichloride, mix the three and stir at 70°C until a uniform transparent liquid is formed to obtain Ternary deep eutectic solvent;

[0050] (2) Pretreatment: Add 0.5g bagasse to the microwave digestion tank, then add 5g ternary deep eutectic solvent, and react at 120°C for 20min; for the accuracy of the experimental data, three parallel experiments were performed for each group of experiments; After completion, immediately put into an ice-water bath to stop the reaction, separate the solid from the liquid, dilute the liquid part by 20 times with distilled water, let it stand, and analyze and measure the sugar content in the reaction solution by HPLC. The solid part was washed with acetone aqueous solution (volume ratio of acetone and water 50:50, v / v) until the filtrate was colorless, and finally the solid part was freeze-dried to obtain pretreated bagasse. The co...

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Abstract

The invention discloses a method for preparing nanocellulose microfibrils through pretreatment of a ternary eutectic solvent, which belongs to the technical field of biomass nanocellulose preparation. The method comprises the following steps of firstly, pretreating lignocellulose biomass by using a ternary eutectic solvent, and separating to obtain a component rich in cellulose, preparing a 1wt% solution from a cellulose-rich component, centrifuging to obtain a nanocellulose suspension, carrying out high-strength ultrasonic treatment to fibrillate nanofibers, and freeze-drying to obtain the nanocellulose microfibril. The particle size range of the prepared nanocellulose microfibril is 26.84-61.26 nm, the removal rate of lignin reaches 56.28%, the effect is remarkable, operation is easy, the condition is mild, the cost is low, and pollution is small; and meanwhile, the used eutectic solvent is very environment-friendly, meets the standard of green chemical production, and has a relatively good practical application value.

Description

technical field [0001] The invention belongs to the technical field of biomass nanocellulose preparation, and in particular relates to a method for preparing nanocellulose microfibrils by pretreatment of a ternary deep eutectic solvent. Background technique [0002] Energy is the basis for human survival and an important pillar for the development of modern society. At present, the excessive development and use of traditional fossil fuels such as coal, oil, and natural gas have caused resource scarcity and also brought a series of environmental problems. Therefore, the sustainable development of new energy has become the top priority of energy work in the new era. Cellulose is one of the most widely distributed and abundant renewable resources in nature. It not only has the advantages required for biomaterials such as renewability, biocompatibility, degradability and non-toxicity, but also has good mechanical properties. Based on this, cellulose has become an important raw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C5/00
CPCD21C5/00
Inventor 周存山姬青华余筱洁张磊涂姗姗
Owner JIANGSU UNIV
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