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A method for simultaneous preparation of nanocellulose assisted by ultrasound and microwave

A nanocellulose and ultrasonic technology, applied in the direction of raw material separation, can solve problems such as rare reports and achieve the effect of rapid preparation

Inactive Publication Date: 2015-10-14
FUJIAN AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, the ultrasonic-microwave joint auxiliary technology has developed rapidly, especially in the field of chemical reaction, extraction and separation, which has attracted the attention of many scientific researchers. The synergistic effect can further strengthen the chemical process, but its application in the field of preparing biomass nanomaterials is rarely reported

Method used

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  • A method for simultaneous preparation of nanocellulose assisted by ultrasound and microwave
  • A method for simultaneous preparation of nanocellulose assisted by ultrasound and microwave
  • A method for simultaneous preparation of nanocellulose assisted by ultrasound and microwave

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preparation example Construction

[0019] The preparation method of nanocellulose of the present invention comprises acid hydrolysis of plant cellulose, centrifugal recovery of liquid acid, centrifugal separation of nanocellulose; specifically comprises the following steps:

[0020] 1) Acid hydrolysis of plant cellulose: Take 0.5-3.0g of plant fiber material as raw material, mix it with liquid acid with a mass concentration of 10-60% and a volume of 40-60mL, place it in an ultrasonic-microwave co-extractor, Under -80℃ and ultrasonic-microwave assisted hydrolysis reaction for 0.5-2.0h and then ready for use.

[0021] 2) Centrifugal recovery of liquid acid: centrifuge the mixture in step 1) at 4000-7000rad / min for 5-10min, and the collected supernatant is the liquid acid solution, which can be recycled after the water is removed by rotary evaporation. Solid phase spare.

[0022] 3) Centrifugal separation of nanocellulose: Mix the solid phase product of step 2) with 50-200mL deionized water, adjust the pH value t...

Embodiment 1

[0024] A method for simultaneously assisting the preparation of nanocellulose by ultrasonic waves and microwaves, comprising the following steps:

[0025] 1) Acid hydrolysis of plant cellulose: Take 0.5g of filter paper fragments and mix them with 50% mass concentration and 40mL of sulfuric acid, and then use ultrasonic-microwave at 65°C in an ultrasonic-microwave combined extraction apparatus (ultrasonic: 40KHz, 50W; microwave: 2450MHz, 10-800W automatically adjusted according to the set temperature) and auxiliary reaction for 1.5h before standby.

[0026] 2) Centrifugal recovery of liquid acid: centrifuge the mixture in step 1) at 6000rad / min for 7min, and the collected supernatant is the sulfuric acid solution, which can be recycled after the water is removed by rotary evaporation, and the solid phase at the bottom is ready for use.

[0027] 3) Centrifugal separation of nanocellulose: Mix the solid phase product of step 2) with 100 mL of deionized water, adjust the pH value...

Embodiment 2

[0029] A method for simultaneously assisting the preparation of nanocellulose by ultrasonic waves and microwaves, comprising the following steps:

[0030] 1) Acid hydrolysis of plant cellulose: take 1.5g of wood pulp fiber and 55% mass concentration of phosphoric acid, 50mL of phosphoric acid fully mixed, in the ultrasonic-microwave combined extraction apparatus at 60 ℃ ultrasonic-microwave (ultrasonic: 40KHz, 50W; microwave : 2450MHz, 10-800W is automatically adjusted according to the set temperature) and the auxiliary reaction is 2.0h later.

[0031] 2) Centrifugal recovery of liquid acid: centrifuge the mixture in step 1) at 5000rad / min for 8min, and the collected supernatant is the phosphoric acid solution, which can be recycled after the water is removed by rotary evaporation, and the bottom solid phase is ready for use.

[0032] 3) Centrifugal separation of nanocellulose: Mix the solid phase product of step 2) with 150 mL of deionized water, adjust the pH value to neutra...

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Abstract

The invention discloses a method for preparing nano cellulose by simultaneous assistance of ultrasonic waves and microwaves, belonging to the field of biomass nano materials. According to the nano material, liquid acid is taken as a catalyst, and the high-efficiency hydrolysis at the amorphous area of cellulose is promoted due to the simultaneous assistance of the ultrasonic waves and microwaves, so that the nano cellulose is rapidly prepared by plant fiber raw materials. The preparation method comprises the steps of acid hydrolysis of plant cellulose, centrifugal recovery of liquid acid and centrifugal separation of nano cellulose. According to the method, the mechanical dispersion action and ultrasonic cavitation effect of the ultrasonic waves, microwave uniform heating effect, catalytic action of the liquid acid and the synergistic effect of the ultrasonic waves and microwaves are utilized sufficiently, and the hydrolytic process of cellulose is enhanced, so that the high-efficiency and rapid preparation of the nano cellulose can be realized. The prepared nano cellulose material can be used for food additives, drug excipients, engineering material additives, specialty paper additives and the like.

Description

technical field [0001] The invention relates to a method for simultaneously assisting the preparation of nanocellulose by ultrasonic waves and microwaves, and belongs to the field of biomass nanomaterials. Background technique [0002] Nanocellulose usually refers to polymer cellulose with a size of 1-100 nm in a certain dimension of space. Compared with natural cellulose, nanocellulose crystals have many excellent properties, such as larger specific surface area, high crystallinity, high hydrophilicity, high modulus, high strength, ultrafine structure, and high transparency. Therefore, nanocellulose has good application value in food additives, reinforcing phase of composite materials, preparation of tissue engineering scaffolds and filter media. At present, the preparation methods of nanocellulose are mainly divided into three types: chemical method, physical method and biological method. The chemical method usually uses liquid acid or alkali as a catalyst to prepare nan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21B1/30
Inventor 卢泽湘范立维郑怀玉徐元发廖益强
Owner FUJIAN AGRI & FORESTRY UNIV
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