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Method for preparing ultrasonic alkylated lignosulfonate bio-based surfactant

A lignosulfonate and surfactant technology, applied in chemical instruments and methods, chemical/physical processes, water pollutants, etc., can solve the problem of limited activity of lignosulfonate surfactants, poor molecular structure regularity, Solve the problems of high critical micelle concentration and achieve the effect of improving the reaction activity of alkylation, increasing the content and lowering the cost

Inactive Publication Date: 2014-04-30
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the shortcomings of low reactivity and poor molecular structure regularity of industrial lignosulfonate, solve the problems of limited activity, high critical micelle concentration (CMC) or no obvious CMC of lignosulfonate surfactant obtained in the prior art Problem, the primary purpose of the present invention is to provide a kind of preparation method of the lignosulfonate bio-based surfactant of ultrasonic alkylation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Dissolve 10g sodium lignosulfonate in 100ml distilled water, then adjust the pH value to 2 with concentrated sulfuric acid with a mass concentration of 98%, and stir to fully disperse and dissolve sodium lignosulfonate to obtain sodium lignosulfonate solution ;

[0037] (2) Treat the sodium lignosulfonate solution with 150W, 40KHz ultrasonic waves for 60min at 25°C, cool the ultrasonic reaction liquid naturally, then remove the solvent by distillation under reduced pressure, and dry at a constant temperature of 60°C for 24h to obtain dark brown ultrasonic lignosulfonate sodium;

[0038] (3) Dissolve ultrasonic sodium lignosulfonate in a mixed solution of 100ml organic solvent and water (obtained from isopropanol and water at a volume ratio of 50:50), and then adjust the pH value with 1mol / L sodium hydroxide solution To 10, stir to fully dissolve the ultrasonic lignosulfonate;

[0039] (4) Add 2g of 1-bromododecane as the alkylating agent and 1g of pyridine as the ...

Embodiment 2

[0044] (1) Dissolve 10 g of sodium lignosulfonate in 100 ml of distilled water and stir to fully disperse and dissolve the sodium lignosulfonate to obtain a sodium lignosulfonate solution.

[0045] (2) Treat the sodium lignosulfonate solution with 300W, 20KHz ultrasonic wave at 30°C for 60min, and cool the ultrasonic reaction liquid naturally, then remove the solvent by distillation under reduced pressure, and dry at a constant temperature of 60°C for 24h to obtain dark brown ultrasonic sodium lignosulfonate .

[0046] (3) Dissolve ultrasonic sodium lignosulfonate in 100ml of a mixed solution of organic solvent and water (obtained from isopropanol and water at a volume ratio of 70:30), and then adjust the pH value with 1mol / L sodium hydroxide solution Adjust to 11, stir to fully dissolve the ultrasonic lignosulfonate;

[0047] (4) Add 2g of 1-bromododecane as the alkylating agent and 1g of pyridine as the catalyst. Under the protection of nitrogen, condense and reflux at abo...

Embodiment 3

[0052] (1) Dissolve 10g sodium lignosulfonate in 100ml distilled water, then adjust the pH value to 0 with concentrated sulfuric acid with a mass concentration of 98%, stir to fully disperse and dissolve sodium lignosulfonate to obtain sodium lignosulfonate solution .

[0053] (2) Treat the sodium lignosulfonate solution with 150W, 40KHz ultrasonic waves at 25°C for 120min, and cool the ultrasonic reaction solution naturally, then remove the solvent by distillation under reduced pressure, and dry at a constant temperature of 60°C for 24h to obtain dark brown ultrasonic sodium lignosulfonate .

[0054] (3) Dissolve ultrasonic sodium lignosulfonate in 100ml of a mixed solution of organic solvent and water (obtained from isopropanol and water at a volume ratio of 20:80), and then adjust the pH value with 1mol / L sodium hydroxide solution Adjust to 12, stir to fully dissolve the ultrasonic lignosulfonate;

[0055] (4) Add 2g of 1-bromododecane as the alkylating agent and 2g of py...

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Abstract

The invention discloses a method for preparing an ultrasonic alkylated lignosulfonate bio-based surfactant, which belongs to the field of lignosulfonate alkylated synthesized surfactant. According to the method, the number of active groups of lignosulfonate is increased and the tidiness of the molecular structure is improved by using an environment-friendly and efficient ultrasonic wave activation technique, the defects that the industrial lignosulfonate is low in reaction activity and poor in tidiness of the molecular structure are overcome; the bio-based surfactant is synthesized from the lignosulfonate through alkylation in a mixture solution system of alkali organic solvents and water in the presence of pyridine and derivatives of pyridine serving as catalysts. The surface tension force of an aqueous solution of the bio-based surfactant with the mass concentration of 1% is as low as 28.2mN / m, and the critical micelle concentration is 5*10<-5>g / L. The surfactant has the advantages of low cost and characteristics of chemical environment-friendless, is possibly used for completely or partially replacing a petroleum base surfactant to be applied to daily chemical fields and is wide in application prospect.

Description

technical field [0001] The invention belongs to the field of lignosulfonate alkylation synthesis of surfactants, in particular to a preparation method of ultrasonic alkylation lignosulfonate bio-based surfactants. Background technique [0002] Lignosulfonate is a derivative of lignin, the second most abundant biomass resource in nature, which is abundant in nature and biorenewable. At the same time, lignosulfonate is the main waste and pollutant in the acid paper pulping industry, with low price and sufficient supply. In the context of increasingly scarce oil resources and high prices, the preparation of lignosulfonate bio-based surfactants through modification is used in industrial and agricultural production and life, such as lignosulfonate concrete water reducers, coal water slurry additives, Pesticide dispersants, ink and dye dispersants, carbon nanotube dispersants, and daily chemical surfactants all have huge potential and competitive advantages. Broadening the utili...

Claims

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Application Information

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IPC IPC(8): C08H7/00B01F17/50C10L1/24C04B24/18B01J20/24C02F1/28C04B103/30C02F101/20C09K23/50
Inventor 沈敏敏周宝文哈成勇邓莲丽孙淳宁胡志忠
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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