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A method for preparing cellulose nanofibrils by pretreatment of deep eutectic solvent

A technology of deep eutectic solvent and nanofibrils, which is applied in cellulose raw material pulping, cellulose pulp post-treatment, fiber raw material treatment, etc., can solve the limitations of large-scale commercial production of CNF, environmental pollution of reaction products, and processing costs Advanced problems, to achieve the effect of low cost, environmental friendliness and simple operation

Active Publication Date: 2021-01-08
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these chemical pretreatments have good effects on agricultural and forestry biomass raw materials, the processing costs are relatively high, and the reaction products will pollute the environment, which seriously limit the large-scale commercial production of CNF.

Method used

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  • A method for preparing cellulose nanofibrils by pretreatment of deep eutectic solvent
  • A method for preparing cellulose nanofibrils by pretreatment of deep eutectic solvent
  • A method for preparing cellulose nanofibrils by pretreatment of deep eutectic solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) Oven drying: oven-dry poplar finished chemical pulp at 40-45°C for 6-7 hours;

[0054] (2) Deep eutectic solvent treatment: the deep eutectic solvent synthesized by choline chloride and urea with a molar ratio of 1:2 was put into a molten state in an oil bath at 100°C, and the dried poplar chemical pulp was added for constant temperature treatment for 2 hours. Obtain mixed solution, wherein the massfraction of poplar chemical pulp in mixed solution is 1%;

[0055] (3) Poplar chemical pulp fiber after separation treatment: after deep eutectic solvent treatment, water is added in the reaction system to terminate the reaction, and then the poplar chemical pulp fiber in the mixed solution is separated;

[0056] (4) High-pressure homogeneous micro-jet treatment: the poplar chemical pulp fiber isolated in step (3) is mixed with a pulp concentration of 0.3%, and then processed by high-pressure homogeneous micro-jet, and the number of times of treatment is 5 times;

[0057] ...

Embodiment 2

[0060] (1) Oven drying: oven-dry poplar finished chemical pulp at 50-55°C for 5-6 hours;

[0061] (2) Deep eutectic solvent treatment: the deep eutectic solvent synthesized by choline chloride and urea with a molar ratio of 1:2 was put into a molten state in an oil bath at 100°C, and the dried poplar chemical pulp was added for constant temperature treatment for 2 hours. Obtain mixed solution, wherein the massfraction of poplar chemical pulp in mixed solution is 1%;

[0062] (3) Poplar chemical pulp fiber after separation treatment: after deep eutectic solvent treatment, water is added in the reaction system to terminate the reaction, and then the poplar chemical pulp fiber in the mixed solution is separated;

[0063] (4) High-pressure homogeneous micro-jet treatment: the poplar chemical pulp fiber isolated in step (3) is prepared into a pulp concentration of 0.3%, and then processed by high-pressure homogeneous micro-jet, and the number of treatments is 10 times;

[0064] (5...

Embodiment 3

[0067] (1) Oven drying: oven-dry poplar finished chemical pulp at 60-65°C for 4-5 hours;

[0068] (2) Deep eutectic solvent treatment: the deep eutectic solvent synthesized by choline chloride and urea with a molar ratio of 1:3 was put into a molten state in an oil bath at 110°C, and the dried poplar chemical pulp was added for constant temperature treatment for 2 hours. Obtain mixed solution, wherein the massfraction of poplar chemical pulp in mixed solution is 1%;

[0069] (3) Poplar chemical pulp fiber after separation treatment: after deep eutectic solvent treatment, water is added in the reaction system to terminate the reaction, and then the poplar chemical pulp fiber in the mixed solution is separated;

[0070] (4) High-pressure homogeneous micro-jet treatment: the poplar chemical pulp fiber isolated in step (3) is mixed with a pulp concentration of 0.3%, and then processed by high-pressure homogeneous micro-jet, and the number of times of treatment is 15 times;

[007...

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Abstract

The invention discloses a method for preparing cellulose nano filaments with the pretreatment of a low-eutectic solvent. The method comprises the following steps: S1, performing the pretreatment withthe low-eutectic solvent: adding chemical slurry into the low-eutectic solvent, and obtaining a mixed solution; S2, separating treated paper pulp fibers: adding water into a reaction system of step S1to terminate the reaction, and separating the paper pulp fibers from the mixed solution; and S3: performing high-pressure homogenization micro-jet treatment: preparing the paper pulp fibers separatedin step S2 into a pulp solution of a given pulp concentration, then performing the high-pressure homogenization micro-jet treatment, spray drying, and obtaining a cellulose nano filament product. Themethod is mild in preparation conditions, simple in operation, low in cost and small in pollution; and the used low-eutectic solvent can be recovered by virtue of a rotary evaporation method so as tobe continuously circularly used, so that the method is environmentally friendly, capable of meeting a green chemical production standard, and good in practical application value.

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 by pretreatment with a deep eutectic solvent. Background technique [0002] The traditional non-renewable resources such as oil and coal on the earth are increasingly depleted, and the sustainable development of energy has become the focus of the world's attention. Cellulose is one of the most abundant natural renewable resources on the earth. It has the advantages of low price, biodegradability, and homogeneity. It has become an important raw material for traditional industries such as pulp and paper, textiles, polymer materials, and medicine. Therefore, how to efficiently develop and utilize renewable resources such as cellulose has become an important issue in the sustainable development strategy of the world today. [0003] In recent years, cellulose nanofibrils (CNFs) have attracted worldwide attenti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C3/00D21C9/00D21C9/18
CPCD21C3/003D21C9/00D21C9/18
Inventor 和铭杨桂花陈嘉川刘昭祥齐乐天
Owner QILU UNIV OF TECH
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