Method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from oil-tea camellia husk

A nanocrystal and nanofiber technology is applied in the field of preparation of nanocellulose, which can solve the problems of high energy consumption, high energy consumption and high production cost by mechanical methods, reduce energy consumption, overcome low product yield, and facilitate the technological process. Effect

Pending Publication Date: 2021-06-22
JIANGNAN UNIV
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Problems solved by technology

Cellulose nanofibers (CNF) are usually prepared by mechanical methods, such as high-pressure homogenization, ultrasound, ball milling, etc., but the mechanical method consumes a lot of energy and the production cost is high.
Chinese patent CN107190546B discloses a method for preparing nano-fibrillar cellulose with high aspect ratio by using Camellia oleifera husk. The cellulose is oxidized by TEMPO / NaClO / NaBr, and then the nano-fibrillar cellulose is obtained through high-pressure homogeneous treatment. The homogeneous pressure is 20-30kpsi (about 138-207MPa), which requires a lot of energy consumption and increases the production cost

Method used

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  • Method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from oil-tea camellia husk

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Embodiment 1

[0033] refer to figure 1 , a method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from Camellia oleifera, the specific steps are:

[0034] S1. Mechanical treatment: take 100g of Camellia oleifera, dry and pulverize, and pass through a 40-mesh sieve;

[0035] S2. Alkali washing: take 50 g of Camellia oleifera powder obtained in step S1, add 750 mL of 2% NaOH solution, heat in a water bath to 80 ° C, and stir for 2 hours at the same time, filter after the reaction is completed, rinse the filter residue with deionized water, and repeat the alkali washing 4 times , wash the filter residue with water until neutral, and dry at 50°C;

[0036] S3. Bleaching: take 20g of the filter residue obtained in step S2, add 300mL of 1.7%NaClO 2 solution, adjust the pH to 3.5, heat in a water bath to 80°C, and stir for 6 hours at the same time, filter after the reaction, wash the filter residue with water until neutral, and dry at 50°C to obtain the crude fiber of...

Embodiment 2

[0045] A method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from Camellia oleifera, the specific steps are:

[0046] S1. Mechanical treatment: take 100g of Camellia oleifera, dry and pulverize, and pass through a 60-mesh sieve;

[0047] S2. Alkali washing: take 50 g of Camellia oleifera powder obtained in step S1, add 1000 mL of 4% NaOH solution, heat it in a water bath to 90 ° C, and stir for 2 hours at the same time, filter after the reaction, rinse the filter residue with deionized water, and repeat the alkali washing 3 times , wash the filter residue with water until neutral, and dry at 50°C;

[0048] S3. Bleaching: take 20g of the filter residue obtained in step S2, add 600mL of 1.5%NaClO 2 solution, adjust the pH to 3.0, heat in a water bath to 90°C, and stir for 4 hours at the same time, filter after the reaction, wash the filter residue with water until neutral, and dry at 50°C to obtain the crude fiber of Camellia oleifera;

[0049] ...

Embodiment 3

[0056] A method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from Camellia oleifera, the specific steps are:

[0057] S1. Mechanical treatment: take 100g of Camellia oleifera, dry and pulverize, and pass through a 40-mesh sieve;

[0058] S2. Alkali washing: take 50 g of Camellia oleifera powder obtained in step S1, add 750 mL of 5% NaOH solution, heat in a water bath to 70 ° C, and stir for 3 hours at the same time, filter after the reaction is completed, rinse the filter residue with deionized water, and repeat the alkali washing 3 times , wash the filter residue with water until neutral, and dry at 50°C;

[0059] S3. Bleaching: take 20g of the filter residue obtained in step S2, add 300mL of 1.5%NaClO 2 solution, adjust the pH to 3.0, heat in a water bath to 70°C, and stir for 6 hours at the same time, filter after the reaction, wash the filter residue with water until neutral, and dry at 50°C to obtain the crude fiber of Camellia oleifera; ...

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Abstract

The invention relates to a method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from oil-tea camellia husk, which comprises the following steps: by taking the oil-tea camellia husk as an initial raw material, firstly carrying out alkali washing and bleaching to obtain crude fibers, carrying out preliminary hydrolysis on the crude fibers by using diluted hydrochloric acid to obtain microcrystalline cellulose, and then carrying out acidolysis on the microcrystalline cellulose by using a sulfuric acid hydrolysis method; washing and centrifuging at a high speed to obtain a cellulose nanocrystal suspension on the upper layer, and further performing high-pressure homogenization on the lower layer to obtain a cellulose nanofiber suspension. According to the method, CNC and CNF are prepared at the same time according to the difference of the crosslinking degree of cellulose, a sparse structure in a cellulose crystalline region is broken into CNC under the action of sulfuric acid, the tightly-combined part in the crystalline region swells through acidolysis, and CNF can be obtained through homogenization under low pressure. The method is beneficial to improving the yield of the oil-tea camellia husk nano cellulose and reducing the production cost of the process.

Description

technical field [0001] The invention relates to a method for preparing nanocellulose, more specifically, to a method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers from Camellia oleifera. Background technique [0002] Camellia oleifera (Camellia oleifera Abel), a plant of the family Theaceae Camellia, is a pure natural high-grade oil plant unique to China. The annual output of camellia oleifera seeds in the country is about 2 million tons, and Camellia oleifera is a by-product of oil processing. The annual output is about 4 million tons Ton. Camellia oleifera contains various chemical components such as lignin, hemicellulose, cellulose, and tea saponin. However, most of the camellia oleifera has not been fully utilized at present, and a large amount of accumulation occupies a lot of land, or it is directly burned in the open, resulting in atmospheric pollution. environmental pollution. [0003] The cellulose content in Camellia oleifera is bet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02D01F2/00D21C5/00
CPCC08B15/02D01F2/00D21C5/00
Inventor 徐化能陈智慧侯洁吕思思
Owner JIANGNAN UNIV
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