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Cellulose nanofibril suspension and preparation method thereof

A technology of nanofibrils and cellulose, which is applied in the direction of cellulose pulp post-treatment, fiber raw material treatment, washing/replacing pulp treatment liquid, etc., which can solve the limitation of nano-cellulose application, has not been widely used, and the processing process is complicated, etc. problems, to achieve the effect of improving oxidation performance, green and environmental protection in the preparation process, and uniform diameter distribution

Active Publication Date: 2021-07-16
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although both acid hydrolysis and oxidation can prepare cellulose nanofibrils, the common problem is that they are all carried out in an aqueous solution system, resulting in poor dispersion of cellulose nanofibrils in organic solvents, such as DMF, Acetonitrile, etc., which also limits the further application of nanocellulose in organic chemistry
[0008] At present, enzymatic hydrolysis is only used as a pretreatment method in the preparation process of cellulose nanofibrils, because the cost of enzymes is high and the treatment process is relatively complicated, it has not been widely used.

Method used

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  • Cellulose nanofibril suspension and preparation method thereof
  • Cellulose nanofibril suspension and preparation method thereof
  • Cellulose nanofibril suspension and preparation method thereof

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preparation example Construction

[0032] The preparation method of a cellulose nanofibril suspension in the present invention comprises putting the wood fiber of 30-40 ° SR in a three-necked flask, and undergoing a polar solvent swelling treatment for 2-4 hours under the condition of an ultrasonic bath at 48-55 °C , and then sequentially add a certain proportion of oxalic acid, sulfuric acid with a volume fraction of 1%, and potassium permanganate for oxidation treatment for 4-6 hours, use hydrogen peroxide to terminate the reaction, and wash the obtained mixed system for 10-30 minutes. Centrifugal treatment, separation The upper liquid, the cellulose nanofibrils suspension with a length of 1-10um and a diameter of 20-60nm in the finally obtained cellulose nanofibril suspension.

[0033] Oxalic acid plays a complex role in the potassium permanganate oxidation system. Under acidic conditions, permanganate ions are oxidized into trivalent manganese ions, but the trivalent manganese ions are not stable, and oxalat...

Embodiment 1

[0038] Take 1g (absolutely dry) coniferous wood fibers with a beating degree of 30°SR in a 500mL three-necked flask, slowly add 45mL of acetone, and seal the flask mouth with a plastic wrap to prevent heat loss and solvent volatilization. The magnetic stirrer is set at 500r / min, put the system in an ultrasonic constant temperature water bath at 50°C, and treat it for 120 min to make the fibers evenly dispersed. Add 2.5g oxalic acid, 100mL sulfuric acid with a volume fraction of 1%, and slowly add potassium permanganate. After adding 1.5g, the system becomes a purple viscous liquid; react for 4 hours, add 4mL hydrogen peroxide dropwise to the system, and the color of the system gradually changes White. Divide the cooled viscous liquid into six equal parts and put them into centrifuge tubes, set the centrifugal speed to 5800r / min, and the centrifugation time to 10min, wash with deionized water 4 times until the supernatant is cloudy, and obtain a length of 8-10μm and a diameter...

Embodiment 2

[0041] Take 1g (absolutely dry) coniferous wood fiber with a beating degree of 35°SR in a 500mL three-necked flask, slowly add 45mL of DMF, seal the flask with plastic wrap, set the magnetic stirrer at 500r / min, and place the system at 50°C In the ultrasonic constant temperature water bath, treat for 120min to make the fibers disperse evenly. Add 2.5g of oxalic acid, 100mL of sulfuric acid with a volume fraction of 1%, and slowly add potassium permanganate. After adding 1.403g, the system becomes a brown viscous liquid; react for 4 hours, add 1.5mL of hydrogen peroxide dropwise to the system, and the system gradually becomes for white. Divide the cooled viscous liquid into six equal parts and put them into centrifuge tubes, set the centrifugal speed to 5800r / min, and the centrifugation time to 10min, wash with deionized water for 5 times until the supernatant becomes turbid, and obtain a tube with a length of 4-6μm and a diameter of 30-40 nm nanofibril suspension.

[0042] S...

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Abstract

The invention provides a cellulose nanofibril suspension and a preparation method thereof, and the method comprises the following steps: step 1, swelling wood fibers in a polar solvent for 2-4 hours to obtain a mixed system A; step 2, sequentially adding oxalic acid, sulfuric acid and potassium permanganate the mixed system A, performing oxidation treatment for 4-6 h, and obtaining a mixed system; and step 3, washing the mixed system B, centrifuging, and separating supernatant liquid to obtain the cellulose nanofibril suspension. According to the method, the complete lattice structure of the cellulose is reserved as far as possible, the problem of uniform dispersion of the cellulose nanofibrils in part of the organic solvent can be solved while the size of the cellulose nanofibrils can be effectively adjusted and controlled, and continuous operation can be realized in the whole process.

Description

technical field [0001] The invention belongs to the field of biopolymer nanomaterials, in particular to a cellulose nanofibril suspension and a preparation method thereof. Background technique [0002] In recent years, with the development of the cellulose field, cellulose, as an important raw material for the papermaking industry, is not only applicable to the traditional papermaking field, but also includes industries such as medical care, agriculture, logistics, transportation and packaging. A series of cellulose-based functional materials and high-performance composite materials can be prepared from special paper made of cellulose through modification and nanometerization. Therefore, cellulose, as a renewable resource with abundant content, maximizes its utilization, and realizes a permanent substitute for non-renewable resources while meeting the requirements of green environmental protection. [0003] In a broad sense, nanocellulose refers to cellulose with at least o...

Claims

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Application Information

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IPC IPC(8): D21C9/00D21C9/02
CPCD21C9/002D21C9/00D21C9/02
Inventor 张素风林瑞刘亚丽唐蕊华李磊
Owner SHAANXI UNIV OF SCI & TECH
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