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Preparation method for nano-cellulose

A nanocellulose and fiber technology, applied in the direction of pulping with organic solvents, etc., can solve the problems of chemical recovery, energy consumption, dehydration ability deterioration, etc. the effect of

Active Publication Date: 2014-09-17
GOLD EAST PAPER JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method consumes a lot of energy in the process of refining / beating plant fiber raw materials; on the other hand, the dehydration ability of pulp with low freeness is deteriorated after TEMPO oxidation, which is not conducive to the separation of oxidation wastewater and the recovery of chemicals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Get 360g softwood chemical pulp fiber (dry pulp) and place it in a trough beater, after dispersing for 30min, add 2g of TEMPO, 24g of NaBr, 60ml of NaClO solution (mass percentage concentration is 10%, contains about 6.6 g absolute dry NaClO), apply 2kg mound for beating, and separate the oxidized fiber and waste water when the freeness of the slurry is 295ml after 190min. After washing 4 times, the oxidized fiber was further beaten to a freeness of 50ml, and the carboxyl content of the obtained oxidized fiber was 0.21mmol / g. The oxidized fiber was nano-treated at 90MPa for 28 passes using a high-pressure homogenizer to obtain a uniform and transparent nanocellulose solution. .

[0030] Compared with the comparative example, the energy consumption of defibrating pretreatment in this embodiment is reduced by 20.8%, and the energy consumption of nano-processing is reduced by 20%.

[0031] Note: Because the example and the comparative example use the same beating equipmen...

Embodiment 2

[0033] Get 360g softwood chemical pulp fiber (absolutely dry pulp) and place it in a trough beater. After dispersing for 30min, add 2g of TEMPO, 24g of NaBr, and 1250ml of NaClO solution (mass percentage concentration is 10%, containing about 137.5 g absolute dry NaClO), apply 2kg weight for beating, and separate the oxidized fiber and waste water when the freeness of the slurry is 305ml after 120min. After washing 4 times, the oxidized fiber was continuously beaten until the freeness was 50ml, and the carboxyl content of the obtained oxidized fiber was 0.82mmol / g. The oxidized fiber was nano-treated at 90MPa for 12 passes using a high-pressure homogenizer to obtain a uniform and transparent nanocellulose solution. .

[0034] Compared with the comparative example, the energy consumption of the defibrating pretreatment in this embodiment is reduced by 50%, and the energy consumption of the nano-processing is reduced by 85.7%.

Embodiment 3

[0036] Get 360g conifer chemical pulp fiber (dry pulp) and place it in a trough beater. After dispersing for 30min, add 2g of TEMPO, 24g of NaBr, and 2500ml of NaClO solution (mass percentage concentration is 10%, containing about 275g Dry NaClO), apply 2kg mound for beating, and separate the oxidized fiber and waste water when the freeness of the slurry is 240ml after 45min. After washing 4 times, the oxidized fiber was further beaten to a freeness of 50ml, and the carboxyl content of the obtained oxidized fiber was 1.45mmol / g. The oxidized fiber was nano-treated with a high-pressure homogenizer at 90MPa for 3 passes to obtain a uniform and transparent nanocellulose solution.

[0037] Compared with the comparative example, the energy consumption of the defibrating pretreatment in this embodiment is reduced by 81.3%, and the energy consumption of the nano-processing is reduced by 91.4%.

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Abstract

The invention relates to a preparation method for nano-cellulose. The method comprises the steps of: providing a plant fiber pulp; untwining the plant fiber pulp to separate the plant fiber into single fiber; conducting pre-defiberization treatment on the untwined plant fiber pulp, and simultaneously adding a TEMPO catalytic oxidation system to oxidize the fiber; when the freeness of the plant fiber pulp reaches 150-450ml, separating the oxidized fiber and wastewater; conducting defiberization treatment on the oxidized fiber again to freeness of 50ml and below, thus obtaining defiberized oxidized fiber; and carrying out nanocrystallization treatment on the defiberized oxidized fiber so as to obtain a nano-cellulose solution. The method is easier to realize wastewater separation and recovery of chemicals, at the same time can save pulping energy consumption by 20%-82%, and is easier to obtain nano-cellulose with uniform size and low cost.

Description

technical field [0001] The invention relates to a method for preparing nanocellulose. Background technique [0002] Nanocellulose fibers refer to fibers whose cross-section is nanometer-sized, and its cross-sectional diameter is generally less than 100 nm. Nanocellulose has a large specific surface area and high mechanical strength properties, and has different properties from natural plant fibers. It can be used as a drug carrier, dispersant, membrane material and nanocomposite reinforcement. At present, nanocellulose mainly includes nanocellulose crystals (NCC) prepared by chemical methods (inorganic acid hydrolysis), or nanofibrillated cellulose (NFC) prepared by mechanical methods. The method of preparing NCC with inorganic acids (hydrochloric acid, sulfuric acid) has a very low yield (about 30%) and requires a large amount of acid consumption, resulting in high production costs, high energy consumption, and environmental pollution. However, the size of nanocellulose f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C3/20
Inventor 马朴刘翔飞秦昀昌王仁荣
Owner GOLD EAST PAPER JIANGSU
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