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A kind of method for preparing nano-cellulose suspension by low-temperature hydrothermal

A nanocellulose and suspension technology, which is applied in the field of low-temperature hydrothermal preparation of nanocellulose suspension, can solve the problems of easy carbonization and the like, and achieve the effects of low corrosiveness, small size, and reduction of production cost and energy consumption.

Active Publication Date: 2022-04-05
HUAFANG +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems in the prior art that strong acid is used in the preparation of nanocellulose by hydrothermal method, and the ultra-low acid content requires high temperature reaction and easy carbonization, the present invention provides a method for preparing nanocellulose suspension by low temperature hydrothermal method, which is carried out under low temperature conditions Hydrothermal reaction avoids cellulose carbonization and does not require the use of catalysts such as strong acids

Method used

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  • A kind of method for preparing nano-cellulose suspension by low-temperature hydrothermal
  • A kind of method for preparing nano-cellulose suspension by low-temperature hydrothermal

Examples

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Effect test

Embodiment 1

[0027] Add microcrystalline cellulose to ethanol-water solution, including 3.3 g of microcrystalline cellulose, 15 mL of ethanol, and 50 mL of distilled water. After ultrasonic treatment for 30 min at an ultrasonic power of 300 W, transfer it to a hydrothermal reaction kettle, add 1 g of hydroxylamine hydrochloride, and React at 85°C for 8 hours, then cool to room temperature, add distilled water, wash 3 times, and then centrifuge. The centrifugation conditions are 500r / min and 50min. liquid. The obtained nanocellulose has a diameter of about 10-50nm and a length of 50-500nm.

Embodiment 2

[0029] Add microcrystalline cellulose to the ethanol-water solution, including 4.0g of microcrystalline cellulose, 15mL of ethanol, and 50mL of distilled water. After ultrasonic treatment for 50min under the condition of ultrasonic power of 100W, transfer it to a hydrothermal reaction kettle, add 1.5g of hydroxylamine hydrochloride, Under neutral conditions, react at 95°C for 8h and then cool down. Distilled water was added to the residue, washed 3 times, and then centrifuged. The centrifugal separation conditions were 1000r / min and 30min. The collected supernatant was the nanocellulose suspension. The obtained nanocellulose has a diameter of about 10-50nm and a length of 50-500nm.

Embodiment 3

[0031] Add microcrystalline cellulose to ethanol-water solution, wherein 2 g of microcrystalline cellulose, 10 mL of ethanol, and 50 mL of distilled water are sonicated for 30 min under the condition of ultrasonic power of 200 W, and then transferred to a hydrothermal reaction kettle, 0.8 g of hydroxylamine hydrochloride is added, and React under neutral conditions at 105°C for 7.5h and then cool. Distilled water was added to the residue, washed 3 times, and then centrifuged. The centrifugal separation conditions were 1000 r / min and 30 min. The separated supernatant was collected to obtain the nanocellulose suspension. The obtained nanocellulose has a diameter of about 10-50nm and a length of 50-500nm.

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Abstract

The invention relates to the technical field of nanofiber preparation, in particular to a method for preparing nanocellulose suspension by low-temperature hydrothermal method. In the method, cellulose raw materials are added to an ethanol-water solution, ultrasonically treated, and a catalyst is added at a temperature of 85-115°C. The reaction is carried out under the following conditions, and the nanocellulose suspension is obtained after post-treatment. This method utilizes the characteristics that the boiling point of ethanol-water solution is lower than water, and uses ethanol-water solution instead of water as solvent to solve the problem of easy carbonization of cellulose caused by high hydrothermal temperature; uses hydroxylamine hydrochloride as catalyst, avoiding strong acid, oxidizing agent, etc. It has broad prospects for industrial application.

Description

technical field [0001] The invention relates to the technical field of nanocellulose preparation, in particular to a low-temperature hydrothermal preparation method for nanocellulose suspension. Background technique [0002] Cellulose is one of the most abundant natural polymers in nature. Among them, nanocellulose has broad application prospects in the field of materials due to its high mechanical properties and low thermal expansion coefficient. According to the length, nanocellulose can be divided into nanocrystalline cellulose / cellulose nanocrystal and cellulose nanofiber. [0003] The commonly used preparation method of nanocellulose is hydrothermal method. When preparing nanocellulose by hydrothermal method, a small amount of hydrochloric acid, hydrochloric acid, etc. are used as catalysts, but strong acid is highly corrosive to equipment, and the treatment of waste acid will cause environmental pollution; or ultra-low acid content (acid mass fraction is 0.05 -0.1%),...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/03C08L1/04
CPCC08J3/03C08J2301/04
Inventor 孙红玉闫英山邓慧王力民盛春英郭春辉田峰任晓宁王光星刘晓敏赵姗姗刘玉玺
Owner HUAFANG