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Carboxymethylated cellulose nanofibril and preparation method thereof

A technology of carboxymethylation and nanofibrils, which is applied in the field of nanocellulose preparation, can solve the problems of poor dispersion and high cost, and achieve the effect of not easy to agglomerate, low cost and good dispersion

Inactive Publication Date: 2018-08-17
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems of high cost and poor dispersibility in the existing mechanical method for preparing nanocellulose, the inventors provided a carboxymethylated cellulose nanofibril and its preparation method after long-term technical and practical exploration. This application adopts carboxylation modification pretreatment before nano treatment, and at the same time optimizes the process conditions and parameters in the preparation process, thereby reducing energy consumption and improving the yield and quality of carboxymethylated cellulose nanofibrils. Broad prospects for industrial application

Method used

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  • Carboxymethylated cellulose nanofibril and preparation method thereof
  • Carboxymethylated cellulose nanofibril and preparation method thereof
  • Carboxymethylated cellulose nanofibril and preparation method thereof

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preparation example Construction

[0042] In view of this, in a specific embodiment of the present invention, a kind of preparation method of carboxymethylated cellulose nanofibril is provided, and described method comprises:

[0043] S1. Material preparation: beating the slurry with a concentration of 1-2%;

[0044] S2. Solution replacement: use absolute ethanol to perform solution replacement treatment on the beaten slurry;

[0045] S3. Carboxymethylation: add the slurry after solution replacement into the mixed solution of isopropanol and NaOH to stir and disperse, then add chloroacetic acid to heat and stir to carry out carboxymethylation reaction on the slurry;

[0046] S4. Nano treatment: Carboxymethylated cellulose nanofibrils are obtained by freeze-drying after high-speed shearing and friction treatment on the carboxymethylated slurry.

[0047] In yet another specific embodiment of the present invention, in the step S1.,

[0048] The pulp is bleached kraft wood pulp, preferably bleached hardwood kraft...

Embodiment 1

[0064] A preparation method of carboxymethylated cellulose nanofibrils, specifically completed according to the following steps: take 40g of dry bleached poplar kraft pulp, tear it into small pieces of 25mm × 25mm, and use a Valli beater to The slurry with a concentration of 1-2% is beaten at a temperature of 20±5°C. When the Canadian Standard Freeness of the slurry was 150ml CSF, the slurry was taken out and dehydrated under reduced pressure. At normal temperature, use absolute ethanol to perform solution replacement treatment on the beaten slurry, the reaction time is 30-45min, and the number of times of solution replacement treatment is 3 times. Add the slurry after solution replacement to the mixed solution of isopropanol and 30% NaOH with a volume ratio of 14:1, stir and disperse for 30-45min, then add 1.5mmol / g chloroacetic acid and heat and stir to carboxymethylate the slurry Reaction, the reaction temperature is 50-60°C, the stirring time is 50-70min, and the stirring...

Embodiment 2

[0066] A preparation method of carboxymethylated cellulose nanofibrils, specifically completed according to the following steps: take 40g of dry bleached eucalyptus kraft pulp, tear it into small pieces of 25mm × 25mm, and use a Valli beater to The slurry with a concentration of 1-2% is beaten at a temperature of 20±5°C. When the Canadian Standard Freeness of the slurry was 150ml CSF, the slurry was taken out and dehydrated under reduced pressure. At normal temperature, use absolute ethanol to perform solution replacement treatment on the beaten slurry, the reaction time is 30-45min, and the number of times of solution replacement treatment is 3 times. Add the slurry after solution replacement to the mixed solution of isopropanol and 30% NaOH with a volume ratio of 14:1, stir and disperse for 30-45min, then add 2.0mmol / g chloroacetic acid and heat and stir to carboxymethylate the slurry Reaction, the reaction temperature is 60-70°C, the stirring time is 50-70min, and the stir...

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Abstract

The invention discloses a carboxymethylated cellulose nanofibril and a preparation method thereof. According to the carboxymethylated cellulose nanofibril and the preparation method thereof, carboxylation modification pre-treatment is adopted before nanocrystallization treatment, meanwhile, the technological conditions and parameters in the preparation process are optimized, and therefore the energy consumption is reduced, meanwhile, the yield of the carboxymethylated cellulose nanofibril is increased, and the quality of the carboxymethylated cellulose nanofibril is improved. Compared with a traditional inorganic acid hydrolysis method, the preparation method has the advantages that no residual acid exists in a preparation system, so that the pollution of the acid to the environment can beavoided, and dialysis can be carried out without lots of water; compared with a mechanical preparation method without chemical pretreatment, the preparation method has the advantages that the preparation conditions are mild, the operation is simple, the cost is low, and the pollution is small; and the method has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of nanocellulose preparation, and in particular relates to a method for preparing cellulose nanofibrils through carboxymethylation pretreatment. Background technique [0002] Nanocellulose refers to cellulose products with a diameter of 1-100 nm and a length of several microns. While having the basic properties of natural cellulose, its nanometer size endows it with a small size effect, so that nanocellulose has many excellent properties, such as light weight, high strength, high Young's modulus, high specific surface area, high reactivity and high And special rheological properties, etc. These characteristics make nanocellulose have great potential application prospects in the fields of papermaking, construction, automobile, food, cosmetics, medicine, coatings and aviation. [0003] Nanocellulose is mainly divided into four categories according to its preparation method, raw material and structure, namely...

Claims

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Application Information

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IPC IPC(8): C08B11/12C08B11/20B82Y40/00
CPCB82Y40/00C08B11/12C08B11/20
Inventor 和铭杨桂花陈嘉川王强
Owner QILU UNIV OF TECH
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