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Preparation method of lignin nano microspheres

A technology of nano-microspheres and lignin, which is applied in the field of preparation of lignin nano-microspheres, can solve the problems of cumbersome pretreatment, maintaining stability, and being difficult for a long time.

Inactive Publication Date: 2020-12-11
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pretreatment of raw lignin is cumbersome, and lignin nanospheres will aggregate after a period of storage, so it is difficult to maintain stability for a long time

Method used

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  • Preparation method of lignin nano microspheres
  • Preparation method of lignin nano microspheres
  • Preparation method of lignin nano microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Get 100ml of self-made black liquor sample, filter through filter paper and remove solid impurities therein, add 900ml of distilled water to dilute to obtain diluent;

[0027] (2) At room temperature, add 2mol / L sulfuric acid to the diluent under agitation, adjust the pH value of the diluent to be 6 and precipitate out at the same time, continue to stir for 30min at room temperature, at a stirring speed of 500rpm, centrifuge (3000r / min) after stirring , 15min) to obtain the first-level precipitate and the first-level supernatant; continue to add 2mol / L sulfuric acid in the first-level supernatant under stirring conditions, adjust the pH value to be 4 and separate out the precipitate simultaneously, and obtain the second-level precipitate and the Secondary supernatant; continue to add 2mol / L sulfuric acid to the secondary supernatant under stirring conditions, adjust the liquid pH value to 2 and precipitate precipitates at the same time, and obtain third-grade precipi...

Embodiment 2

[0032] Compared with Example 1, the difference of Example 2 is that the addition of ultrapure water in the step (4) is 65% of the suspension quality, and it is the same as the operation of Example 1.

[0033]The prepared lignin nano-microspheres were detected, and the dispersion performance of the lignin nano-microspheres was improved.

Embodiment 3

[0035] Compared with Example 1, the difference of Example 2 is that the addition of ultrapure water in step (4) is 70% of the suspension quality, which is the same as in Example 1 with operation.

[0036] Carry out SEM detection to the lignin nano-microsphere that embodiment 3 makes, the result is as follows Figure 1-3 as shown, Figure 1-Figure 3 The lignin nanospheres corresponding to raw material lignin KL1, KL2, KL3 respectively, from Figure 1-3 It can be seen that the lignin nanospheres prepared in this example have high sphericity and good dispersion performance; and with the reduction of the phenolic hydroxyl content of the raw material lignin, the particle size and hollowness of the prepared nanospheres show a gradual decrease. small trend.

[0037] In order to evaluate the stability of lignin nanospheres, the changes of particle size and Zeta potential of lignin nanospheres with time and pH value were detected. After being placed in solutions with different pH va...

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Abstract

The invention discloses a preparation method of lignin nano microspheres. The method comprises the following steps: regulating the pH value of black liquor step by step by using dilute acid such as sulfuric acid and the like, and carrying out fractional precipitation on lignin to obtain raw material lignin with different phenolic hydroxyl contents; and dissolving the raw material lignin in an organic solvent, adding ultrapure water while stirring, and preparing the lignin nanospheres by a self-assembly method. According to the method, the lignin nano-microspheres are prepared by using the green and environment-friendly organic solvent, water is used as a dialyzing agent, reagents can be recycled, no pollution is caused, no solvent is left in the product, and a wide prospect is provided forhigh-valued utilization of lignin; various properties of the prepared lignin nano microspheres are greatly improved, such as stability, dispersibility and the like; and hollow and solid lignin nano microspheres are obtained and can be respectively applied according to the performance, so that the potential application range of lignin is widened.

Description

technical field [0001] The invention belongs to the field of preparation of lignin nanometer materials, and in particular relates to a preparation method of lignin nanometer microspheres. Background technique [0002] Lignin is known as one of the most abundant green resources in the 21st century, accounting for 20%-30% of the total plant mass, and is the second largest biomass polymer raw material. Lignin is composed of guaiacylphenylpropane structural unit, syringylphenylpropane structural unit and p-hydroxyphenylpropane structural unit, three-dimensional space network structure formed by ether bond and carbon-carbon bond. Molecular polymers have very complex chemical structures, and the contents of lignin structural units from different sources are different, and the connection methods are also very different. 40% of the biologically produced energy is present in lignin in terms of enthalpy specific capacity, yet the utilization of lignin is still not widespread. Improv...

Claims

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Application Information

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IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 房桂干严振宇邓拥军沈葵忠
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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