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Preparation method of phenolated lignin amine cationic emulsifier

A cationic emulsifier, phenolic lignin technology, applied in building components, building insulation materials, buildings, etc., can solve the problem that lipophilic and hydrophilic functional groups cannot be introduced, emulsification performance is limited, and the number of alkali lignin active points is limited. And other issues

Active Publication Date: 2015-05-06
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0025] The technical solution of the present invention is aimed at the limitation of the number of active points in alkali lignin, which cannot introduce more lipophilic and hydrophilic functional groups, thus limiting the further improvement of its emulsifying performance

Method used

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  • Preparation method of phenolated lignin amine cationic emulsifier
  • Preparation method of phenolated lignin amine cationic emulsifier
  • Preparation method of phenolated lignin amine cationic emulsifier

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Weigh 100 parts of wood pulp alkali lignin, 20 parts of phenol, 3 parts of sodium hydroxide and 100 parts of water in parts by weight, add them to a three-necked flask with a condenser tube and a thermometer, stir and dissolve, and keep the reaction mixture at a constant temperature of 70 °C After stirring and reacting for 3 hours, it was acidified with 1 mol / L hydrochloric acid to pH=2.5, filtered with suction, and the filter cake was washed with hot water at 80°C until no free phenol existed to obtain phenolated lignin. Dissolve phenolized lignin with 10% NaOH solution and adjust the pH to 10.5, raise the temperature to 90°C, slowly drop in a mixture of 55 parts of diethylenetriamine and 35 parts of 37% formaldehyde, and stir for 4 hours at a constant temperature. After the reaction is finished, it is cooled to obtain a phenolated lignin amine cationic emulsifier solution, which is acidified and mixed with asphalt to make emulsified asphalt which can be used for road c...

Embodiment 2

[0051] Weigh 100 parts of wood pulp alkali lignin, 25 parts of phenol, 4 parts of sodium hydroxide and 200 parts of water in parts by weight, add them to a three-necked flask with a condenser tube and a thermometer, stir and dissolve, and keep the reaction mixture at a constant temperature of 75 °C After stirring and reacting for 2.5 hours, acidify with 1 mol / L hydrochloric acid to pH=2.5, filter with suction, wash the filter cake with 85°C hot water until no free phenol exists, and obtain phenolated lignin. Dissolve the phenolized lignin with 10% NaOH solution and adjust the pH to 11, raise the temperature to 90°C, slowly drop in a mixture of 80 parts of diethylenetriamine and 38 parts of 37% formaldehyde, and stir for 4 hours at a constant temperature. After the reaction is finished, it is cooled to obtain a phenolated lignin amine cationic emulsifier solution, which can be used for waterproof construction of building toilets.

Embodiment 3

[0053] Weigh 100 parts by weight of bamboo pulp alkali lignin, 30 parts of phenol, 5 parts of sodium hydroxide and 300 parts of water into a three-necked flask with a condenser tube and a thermometer, stir and dissolve, and keep the reaction mixture at a constant temperature of 80 °C After stirring and reacting for 2 hours, it was acidified with 1 mol / L hydrochloric acid to pH=2.5, filtered with suction, and the filter cake was washed with hot water at 90°C until no free phenol existed to obtain phenolated lignin. Dissolve the phenolized lignin with 10% NaOH solution and adjust the pH to 11, raise the temperature to 95°C, slowly drop in a mixture of 110 parts of triethylenetetramine and 40 parts of 37% formaldehyde, and stir for 3 hours at a constant temperature. After the reaction is finished, it is cooled to obtain a phenolated lignin amine cationic emulsifier solution, which can be used for road construction.

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Abstract

The invention discloses a preparation method of a phenolated lignin amine cationic emulsifier. The method comprises the following steps: heating an alkaline liquid of alkali lignin and a proper amount of phenol to 70-100 DEG C and reacting for 1-3h, then, acidizing a reaction liquid to realize pH=2.5 with 1 mol / L hydrochloric acid, performing suction filtration, washing with hot water at 80-100 DEG C until free phenol disappears completely, thus obtaining phenolated lignin; dissolving the phenolated lignin in a NaOH liquid with mass fraction of 10% and regulating pH to 10.5-12, then, further adding a mixed liquid of a certain amount of small molecule polyamine and 37% formaldehyde, reacting for 3-5h at 90 DEG C, then, introducing amine methyl hydrophilic groups into the phenolated lignin, thereby obtaining the cationic emulsifier which has positive electricity under the condition of diluted acid. In comparison with the cationic emulsifier modified by the lignin which is not phenolated, the emulsifier provided by the invention has higher surface activity, stronger Zeta potential and stronger emulsion stability, and can be widely used in the fields of road engineering, building waterproofing, material corrosion prevention, water conservancy construction, and so on.

Description

technical field [0001] The invention belongs to the technical field of pulping and papermaking waste liquid recovery and utilization, and in particular relates to a preparation method of a modified alkali lignin amine cationic emulsifier. Background technique [0002] Lignin is a natural phenolic polymer with a three-dimensional structure, and it is the second largest natural organic compound after cellulose in nature. At present, the available industrial lignin mainly comes from the pulp and paper industry, and can be divided into insoluble alkali lignin and soluble lignosulfonate according to different pulping processes. Under the action of alkali, lignin undergoes a certain degree of alkaline hydrolysis to increase its solubility, and is extracted, separated by precipitation, and the obtained lignin is called alkali lignin. The pulp and paper industry worldwide separates about 140 million tons of cellulose from plants each year, while producing about 50 million tons of i...

Claims

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Application Information

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IPC IPC(8): C08H7/00C08J3/03C08L95/00
Inventor 刘祖广安兰芝曹松卢祥雷福厚
Owner GUANGXI UNIV FOR NATITIES
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