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Method for preparing cellulose nanofibril CNF through polyatomic acid treatment

A technology of nanofibrils and polyacids, which is applied in fiber treatment, plant fibers, textiles and papermaking, etc., can solve the problems of high energy consumption, poor product dispersibility, and uneven particle size of CNF, and achieve high yield and high dispersion Good performance and shorten the oxidation treatment time

Inactive Publication Date: 2020-11-24
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The energy consumption of CNF prepared by purely mechanical method is high, and the energy consumption of its preparation is as high as 70MWh / t, which leads to high production cost, and at the same time, there are equipment blockage, low efficiency of spinning broom, serious damage to cellulose structure, and uneven particle size of CNF , poor dispersion and other issues
In response to the above problems, many researchers have developed a series of pretreatment methods, including enzymatic hydrolysis, sulfuric acid hydrolysis, carboxymethylation, TEMPO catalytic oxidation, periodate oxidation, etc. At present, the above pretreatment methods have some shortcomings , such as expensive chemicals used, long preparation reaction time, serious environmental pollution, poor product dispersion, etc., severely limit the industrial production and application of CNF

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In Example 1, hardwood kraft pulp was used as the research object, and CNF was prepared by succinic acid treatment and chlorine dioxide oxidation, and the specific steps were as follows:

[0023] (1). Thawing or breaking up of raw materials: add water to dilute the hardwood kraft pulp to a pulp concentration of 1.0%, and then break it up with a deflaker for 1 min.

[0024] (2). Dehydration of the raw material: the raw material obtained in the above step (1) is filtered and dehydrated to obtain the pretreated raw material.

[0025] (3). Succinic acid treatment of the pretreated raw material: put the pretreated raw material obtained in the above step (2) in a reactor, add water and succinic acid to mix with the raw material, and perform high-temperature short-term treatment. The solid-to-liquid ratio used in the reactor was 1:12, the amount of succinic acid added was 0.3 mol / L, and the mixture in the reactor was subjected to acid hydrolysis at a temperature of 190° C. for...

Embodiment 2

[0032] In Example 2, the hardwood kraft dissolving pulp was used as the research object, and CNF was prepared by citric acid treatment and sodium chlorite oxidation, and the specific steps were as follows:

[0033] (1). Thawing or breaking up of raw materials: Dilute the hardwood kraft dissolving pulp with water to a pulp concentration of 1.5%, and then break it up for 2 minutes with a thinning machine.

[0034] (2). Dehydration of the raw material: the raw material obtained in the above step (1) is filtered and dehydrated to obtain the pretreated raw material.

[0035] (3). Citric acid treatment of the pretreated raw material: the pretreated raw material obtained in the above step (2) is placed in a reactor, and water and citric acid are added to mix with the raw material for high-temperature short-term treatment. The solid-to-liquid ratio used in the reactor was 1:10, the amount of citric acid added was 0.2 mol / L, and the mixture in the reactor was subjected to acid hydrolys...

Embodiment 3

[0042] In Example 3, coniferous wood sulfite pulp was used as the research object, and CNF was prepared by succinic acid treatment and hydrogen peroxide oxidation, and the specific steps were as follows:

[0043] (1). Thawing or breaking up of raw materials: Dilute coniferous wood sulfite pulp with water to a pulp concentration of 1.0%, and then break it up with a beater for 3 minutes.

[0044] (2). Dehydration of the raw material: the raw material obtained in the above step (1) is filtered and dehydrated to obtain the pretreated raw material.

[0045](3). Succinic acid treatment of the pretreated raw material: the pretreated raw material obtained in the above step (2) is placed in a reactor, and water and succinic acid are added to mix with the raw material for high temperature and short-term treatment. The solid-to-liquid ratio used in the reactor was 1:15, the amount of succinic acid added was 0.5 mol / L, and the mixture in the reactor was subjected to acid hydrolysis at a t...

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Abstract

The invention discloses a method for preparing cellulose nanofibrils (CNF) by adopting polyatomic acid high-temperature short-time treatment, and belongs to the field of natural polymer materials. Inthe preparation process of CNF, chemical pulp is used as a raw material, cellulose is decomposed at high temperature for a short time by adopting binary or ternary organic acid, the Zeta potential ofthe cellulose is reduced, and the Zeta potential of the cellulose is further reduced through carrying out oxidation treatment on the pulp subjected to acidolysis; and finally, the oxidized slurry is subjected to high-pressure homogenization treatment, the CNF colloid with high dispersity is obtained, and the Zeta potential of the CNF colloid can reach -40 mV or above. The preparation process has good industrial implementation conditions, and the prepared CNF has the characteristics of high yield (more than 90%), good dispersibility, stable performance, large length-diameter ratio and the like,and has a good application prospect.

Description

technical field [0001] The invention provides a method for preparing CNF by polybasic acid treatment, which has properties such as high yield and good dispersibility. Background technique [0002] Cellulose nanofibrils (CNF) refer to microfibril bundles (clusters) with diameters of nanometers and lengths of hundreds of nanometers or even micrometers. There are both crystalline regions and amorphous regions in the CNF structure, which has the advantages of high hydrophilicity, renewable, easy biodegradation, high reactivity, nano-size effect, etc., and is widely used in food, medicine, automobiles, composite materials, electronic products and oil exploration and other fields. [0003] At present, there are more than ten methods for preparing CNF, among which the most commonly used methods include high-pressure homogenization, microfluidics, and grinding. The energy consumption of CNF prepared by purely mechanical method is high, and the energy consumption of its preparation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/192D06M13/207D06M11/50D06M11/30D06M11/54D06M101/06
CPCD06M13/192D06M13/207D06M11/50D06M11/30D06M11/54D06M2101/06
Inventor 杨秋林徐双侯庆喜霍丹张凤山
Owner TIANJIN UNIV OF SCI & TECH
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