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Lignin-based amphiphilic azo-polymer colloidal spheres as well as preparation method and application thereof

An azo polymer and lignin-based technology, which is applied in the field of derivatives of natural polymer compounds, can solve the problem of high preparation cost of azo polymer colloidal balls, and achieve the effects of improving utilization value, promoting enthusiasm, and reducing preparation cost

Active Publication Date: 2015-04-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a low-cost lignin-based amphiphilic azo polymer colloidal sphere and a preparation method thereof for the high cost of preparation of the existing azopolymer colloidal spheres

Method used

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  • Lignin-based amphiphilic azo-polymer colloidal spheres as well as preparation method and application thereof
  • Lignin-based amphiphilic azo-polymer colloidal spheres as well as preparation method and application thereof
  • Lignin-based amphiphilic azo-polymer colloidal spheres as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 1.8g (containing 6mmol benzene ring unit) alkali lignin, dissolve in 200mL NaOH solution (1.0×10 -4 mol / L), under the condition of 85° C. water bath, 0.32 g of hydrogen peroxide with a mass percentage of 30% was added dropwise, reacted for 1.5 h and then cooled to room temperature to obtain demethoxylized alkali lignin.

[0036] Weigh 0.744g of aniline (8mmol) and dissolve it in 25mL of ethanol, add 10mL of 0.117g / mL dilute sulfuric acid (12mmol) dropwise to the solution, and stir the reaction at 100r / min at 0°C for 20min. Then, under stirring, dropwise add 5mL 0.175g / mLNaNO 2 Solution (8.5mmol), continue to react for 1.5h to obtain the corresponding diazonium salt.

[0037] Mix the oxidized alkali lignin with the diazonium salt prepared above, add 3% NaOH solution to adjust the pH to 10, and stir at 0° C. at 100 r / min to continue the reaction for 1.5 h. 2g / mL sulfuric acid was added dropwise to adjust the pH of the solution to 3, and the product was precipitated b...

Embodiment 2

[0045] Take 1.8g (containing 6mmol benzene ring unit) alkali lignin, dissolve in 200mL NaOH solution (1.0×10 -4 mol / L), under the condition of 95°C water bath, 0.36 g of hydrogen peroxide with a mass percentage of 25% was added dropwise, reacted for 1 hour, and then cooled to room temperature to obtain demethoxylized alkali lignin.

[0046] Weigh 1.112g p-nitroaniline (8mmol) and dissolve it in 30mL ethanol, add 10mL 0.117g / mL dilute sulfuric acid (12mmol) dropwise to the solution, and stir the reaction at 120r / min at 0°C for 20min. Then, under stirring, dropwise add 5mL 0.175g / mLNaNO 2 Solution (8.5mmol), continue to react for 1h to obtain the corresponding diazonium salt.

[0047] Mix the oxidized alkali lignin with the diazonium salt prepared above, add 3% NaOH solution by mass to adjust the pH to 12, and stir at 0°C at 120r / min to continue the reaction for 1h. 2g / mL hydrochloric acid was added dropwise to adjust the pH of the solution to 2, and the product was precipitat...

Embodiment 3

[0052] Take 1.8g (containing 6mmol benzene ring unit) alkali lignin, dissolve in 200mL NaOH solution (1.0×10 -4 mol / L), under the condition of 85° C. water bath, 0.36 g of hydrogen peroxide with a mass percentage of 35% was added dropwise, reacted for 1 hour, and then cooled to room temperature to obtain demethoxylized alkali lignin.

[0053] Weigh 1.11g of p-aminobenzoic acid (8mmol) and dissolve it in 20mL of ethanol, add 10mL of 0.117g / mL dilute sulfuric acid (12mmol) dropwise to the solution, and stir the reaction at 120r / min at 0°C for 20min. Then, under stirring, dropwise add 5mL 0.175g / mLNaNO 2 Solution (8.5mmol), continue to react for 1h to obtain the corresponding diazonium salt.

[0054] The oxidized alkali lignin was mixed with the diazonium salt prepared above, and the pH was adjusted to 9 by adding 3% NaOH solution by mass percentage, and the reaction was continued for 1 h at 0° C. with stirring at 100 r / min. 2g / mL sulfuric acid was added dropwise to adjust the ...

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Abstract

The invention discloses lignin-based amphiphilic azo-polymer colloidal spheres as well as a preparation method and application thereof. The preparation method comprises the following steps of: dissolving alkali lignin in a NaOH solution with pH of 8-14, dropwise adding a hydrogen peroxide solution with the mass concentration of 25%-35% under the condition of a 85-95 DEG C water bath, after reacting for 0.5-1.5 hours, and cooling to a room temperature to obtain the alkali lignin without methoxyl; preparing diazonium salt; mixing the alkali lignin without methoxyl with the diazonium salt, adding an alkalinity conditioning agent to adjust pH to 8-14, after reacting, adding an acidity conditioning agent to adjust pH of the solution to 1-4, so that products are acidified out and precipitated, washing precipitates by deionized water, after drying, taking out, dissolving the products in an organic solvent, and adding water serving as a precipitator to obtain the lignin-based amphiphilic azo-polymer colloidal spheres. The solid content of ceramic slurry prepared from the lignin-based amphiphilic azo-polymer colloidal spheres disclosed by the invention reaches up to 70.9wt%-73.1wt%, and is far higher than that of blank slurry; and compared with a conventional dispersion agent, the lignin-based amphiphilic azo-polymer colloidal spheres have a better dispersion effect.

Description

technical field [0001] The invention relates to lignin treatment, in particular to a lignin-based amphiphilic azo polymer colloidal ball and a preparation method thereof, belonging to the technical field of derivatives of natural polymer compounds. Background technique [0002] The depletion of non-renewable fossil resources and the increasingly prominent environmental problems of papermaking waste liquor make the recovery and utilization of lignin renewable resources in papermaking waste liquor extremely important. Lignin is the second most abundant natural polymer compound in the plant kingdom, accounting for about 20% to 30% of the weight of plants, and is a sustainable natural resource. However, lignin usually does not appear in the form of resources, but is a by-product of the paper industry, which is the main component of paper-making waste liquid. Currently, paper-making waste liquid accounts for 17% of the total industrial wastewater in my country. The development o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C04B35/634
Inventor 邱学青邓永红张伟健楼宏铭庞煜霞杨东杰
Owner SOUTH CHINA UNIV OF TECH
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