Method for increasing content of phenol hydroxyl of lignosulfonate by ultrasonic waves and application

A technology of phenolic sulfonate phenolic hydroxyl group and lignosulfonic acid salt is applied in the field of improving the reaction activity of lignosulfonate, which can solve the problem of low content of phenolic hydroxyl group of reactive groups, limited application scope and use value, and unfavorable mass transfer. and reaction problems, to achieve the effect of short process route, significant ultrasonic effect, and reduction of process cost and equipment cost

Active Publication Date: 2013-05-01
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, lignosulfonate has the following disadvantages: ①The complex three-dimensional network polymer structure of lignosulfonate makes the important active group phenolic hydroxyl group be wound and closed, which is not conducive to mass transfer due to steric hindrance and reaction; ② The content of the important reactive group phenolic hydroxyl group is low, and the reactivity is low, which limits its application range and use value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Dissolve 5g of sodium lignosulfonate in 50ml of distilled water, then adjust the pH value to 0 with concentrated sulfuric acid solution with a mass percentage of 98%, and stir to fully disperse sodium lignosulfonate in the acidic aqueous solution to obtain lignin Sodium sulfonate solution.

[0031] (2) Treat the sodium lignosulfonate solution with 150W, 40kHz ultrasonic wave at 25°C for 60min, cool the ultrasonic reaction solution naturally, then remove the solvent by distillation under reduced pressure, and dry at constant temperature to obtain a dark brown sodium lignosulfonate ultrasonic sample. Taking the phenolic hydroxyl content as the standard, it is measured according to the ultraviolet differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1):213~221.). The phenolic hydroxyl content of lignosulfonate was 0.6553% before ultrasonication, and 1.5785% after ultrasonication, and the ultrasonic efficiency reached 141%.

Embodiment 2

[0036] (1) Dissolve 10g of sodium lignosulfonate in 100ml of distilled water, then adjust the pH value to 2 with concentrated sulfuric acid solution with a mass percentage of 98%, and stir to fully disperse sodium lignosulfonate in the acidic aqueous solution to obtain lignin Sodium sulfonate solution.

[0037] (2) Treat the sodium lignosulfonate solution with 150W, 40kHz ultrasonic waves at 25°C for 60 minutes, and cool the ultrasonic reaction solution naturally, then remove the solvent by distillation under reduced pressure, and dry at constant temperature to obtain a dark brown ultrasonic sodium lignosulfonate sample. Taking the phenolic hydroxyl content as the standard, it is measured according to the ultraviolet differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1):213~221.). After ultrasonication, the phenolic hydroxyl content of lignosulfonate increased from 0.6553% to 1.5539%, and the ultrasonic efficiency reached 137%.

Embodiment 3

[0042] (1) Dissolve 10g of sodium lignosulfonate in 100ml of distilled water, then adjust the pH value to 2 with concentrated hydrochloric acid solution with a mass percentage of 37.5%, and stir to fully disperse sodium lignosulfonate in the acidic aqueous solution to obtain lignin Sodium sulfonate solution.

[0043] (2) Treat the sodium lignosulfonate solution with 150W, 40kHz ultrasonic waves at 30°C for 60 minutes, and cool the ultrasonic reaction liquid naturally, then remove the solvent by distillation under reduced pressure, and dry at constant temperature to obtain a dark brown sodium lignosulfonate sample. Taking the phenolic hydroxyl content as the standard, the phenolic hydroxyl content of lignosulfonate after ultrasonic measurement was increased from 0.6553% to 0.9166% by ultraviolet differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1): 213-221.) , the ultrasonic efficiency is 39.9%.

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Abstract

The invention discloses a method for increasing the content of a phenol hydroxyl of lignosulfonate by ultrasonic waves and application. The method comprises the steps that lignosulfonate is dissolved in water, the pH value of lignosulfonate is regulated to be 0-4, and stirring is performed, so that lignosulfonate is dispersed or dissolved fully, and a lignosulfonate solution is obtained; the ultrasonic waves with a service power ranging between 150W and 300W and a frequency ranging between 20kHz and 40kHz at the temperature ranging between 20 DEGC and 30 DEG C act on the lignosulfonate solution for 60-120min, and natural cooling is performed; and the cooled ultrasonic reaction solution is subjected to reduced pressure distillation and constant-temperature drying, so that lignosulfonate with increased content of the phenol hydroxyl is obtained. The method is mild in reaction condition, low in cost and environment-friendly, can be operated easily, and has a broad application prospect.

Description

technical field [0001] The invention belongs to the field of improving the reactivity of lignosulfonate, and in particular relates to a method and application for increasing the phenolic hydroxyl content of lignosulfonate by using ultrasonic waves. Background technique [0002] Lignosulfonate is a derivative of lignin, the second most abundant biomass resource in nature. Three-dimensional net-like natural macromolecules, rich in nature and bio-renewable. As the largest source of natural aromatic compounds, it has many important uses, including the preparation of phenolic resin as a phenol substitute, or the preparation of natural surfactants and metal ion adsorbents through modification. As a major waste and pollutant in the acid paper pulping industry, lignosulfonates are inexpensive and plentiful. Therefore, widening its utilization range and improving its utilization value are of great significance to solving environmental pollution and protecting the ecological environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/28C08L97/00
Inventor 哈成勇周宝文沈敏敏邱振名张利萍
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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