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Acetylation lignin amphiphilic polymer nanometer colloid sphere and preparation method thereof

A technology of amphiphilic polymers and nano colloids, which is applied in the field of fine chemicals, can solve the problems of restricting the research and large-scale application of lignin colloidal materials, restricting lignin-based colloidal substances, complex preparation methods, etc., achieving good application prospects and Market potential, increased utilization value, strong degradability effect

Active Publication Date: 2013-08-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

About 150 billion tons can be synthesized through photosynthesis of plants on the earth every year; while the annual output of industrial lignin from pulp and paper waste liquid is about 50 million tons, of which less than 10% are effectively utilized, and most of the others are Burned through the alkali recovery device, resulting in a huge waste of resources
High-cost raw materials, complex preparation methods and single micron-sized hollow micelles restrict the application field of lignin-based colloidal materials, and also restrict the research and large-scale application of lignin-based colloidal materials.

Method used

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  • Acetylation lignin amphiphilic polymer nanometer colloid sphere and preparation method thereof
  • Acetylation lignin amphiphilic polymer nanometer colloid sphere and preparation method thereof
  • Acetylation lignin amphiphilic polymer nanometer colloid sphere and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) 0.1g alkaline pulping straw pulp black liquor acid analysis alkali lignin (weight average molecular weight 3640g / mol) is placed in the round bottom flask of 50ml, the mixed solution (alkali of the acetyl bromide of adding 25ml and glacial acetic acid The volume ratio of lignin to acetyl bromide is 1:15), sealed, heated to 50° C. and magnetically stirred for 4 hours to obtain a reaction solution containing acetylated lignin. figure 1 It is the infrared spectrogram of the step acid analysis alkali lignin and the intermediate product acetylated lignin measured by the German Thermo NICOLET 380 infrared spectrophotometer. Such as figure 1 As shown, 1270cm -1 The stretching vibration of the phenolic hydroxyl C-O bond in lignin, 1708cm -1 The stretching vibration of non-conjugated carbonyl in lignin, 1762cm -1 The position is the stretching vibration of the carbonyl after acetylation, indicating that the hydroxyl group in the purified lignin molecule is acetylated, and ...

Embodiment 2

[0032] (1) 0.5g alkaline pulping bamboo pulp black liquor acid analysis alkali lignin (weight average molecular weight 3260g / mol) is placed in the round bottom flask of 50ml, the mixed solution (alkali of the acetyl bromide of adding 25ml and glacial acetic acid The volume ratio of lignin to acetyl bromide is 1:20), sealed, heated to 70° C. and magnetically stirred for 6 hours to obtain a reaction solution containing acetylated lignin.

[0033] (2) The reaction liquid containing acetylated lignin obtained in step (1) is subjected to rotary steaming (the vacuum degree during rotary steaming is 9.0mbar, and the temperature is -10° C.) to obtain acetylated lignin, and the obtained acetylated lignin Dissolve in 5ml tetrahydrofuran to obtain acetylated lignin tetrahydrofuran solution, dilute the solution to a concentration of 4.0g / L with tetrahydrofuran, add 2.5ml distilled water, the weight of distilled water accounts for 33% of the total volume of the solution, stir under normal t...

Embodiment 3

[0035] (1) 0.5g alkaline pulping wood pulp black liquor acid analysis alkali lignin (weight average molecular weight 3500g / mol) is placed in the round bottom flask of 50ml, the mixed solution (alkali of the acetyl bromide of adding 25ml and glacial acetic acid The volume ratio of lignin to acetyl bromide is 1:25), sealed, heated to 55° C. and magnetically stirred for 2.5 hours to obtain a reaction solution containing acetylated lignin.

[0036] (2) The reaction liquid containing acetylated lignin obtained in step (1) is subjected to rotary steaming (the vacuum degree during rotary steaming is 9.0mbar, and the temperature is -10° C.) to obtain acetylated lignin, and the obtained acetylated lignin Dissolve in 5ml tetrahydrofuran to obtain acetylated lignin tetrahydrofuran solution, dilute the solution with tetrahydrofuran to a concentration of 1.0g / L, add 3ml distilled water, the weight of distilled water accounts for 37.5% of the total volume of the solution, stir under normal t...

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Abstract

The invention discloses an acetylation lignin amphiphilic polymer nanometer colloid sphere and a preparation method thereof. The preparation method comprises the following steps of: dissolving 1-5 parts by weight of alkali lignin into 200-500 parts by weight of mixed solutions of glacial acetic acid and acetyl reagents, and heating in water bath at 40-60 DEG C for 2-4 hours; and rotationally evaporating to remove the glacial acetic acid, then adding 250-900 parts by weight of organic solvents to dissolve and dilute acetylation lignin, and adding 100-450 parts by weight of water to change a microfacies environment so as to obtain the acetylation lignin amphiphilic polymer nanometer colloid sphere. The method disclosed by the invention has the advantages of simplicity, rich and low-cost raw material source, reutilization of the glacial acetic acid used in production in large quantities and low production cost; and compared with a micron-scale random sodium lignosulfonate / chitosan micelle and a lignin urea-formaldehyde resin micelle, the prepared acetylation lignin amphiphilic polymer nanometer colloid sphere is a uniform nanoscale hollow spherical micelle, achieves the drug loading capacity of pesticide abamectin higher than 50% and is a green nanometer material.

Description

technical field [0001] The invention relates to an amphiphilic polymer colloid ball, in particular to an acetylated lignin-based amphiphilic polymer nano colloid ball and a preparation method thereof, belonging to the technical field of fine chemicals. technical background [0002] Lignin exists widely in plant cell walls and is the second largest natural polymer compound in land plants after cellulose. About 150 billion tons can be synthesized through photosynthesis of plants on the earth every year; while the annual output of industrial lignin from pulp and paper waste liquid is about 50 million tons, of which less than 10% are effectively utilized, and most of the others are Burned by the alkali recovery device, resulting in a huge waste of resources. Lignosulfonate in acid pulping waste liquor is the main form of lignin application in industry, because its molecule contains hydrophobic skeleton mainly composed of phenylpropane structural unit, hydrophilic sulfonic acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/12C08H7/00C08J9/00
Inventor 邱学青邓永红钱勇杨东杰欧阳新平易聪华
Owner SOUTH CHINA UNIV OF TECH
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