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Method and application of increasing phenolic hydroxyl content of lignosulfonate by using ultrasonic waves

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: 2015-09-02
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 to 0 with a 98% mass percent concentrated sulfuric acid solution, stir to make the sodium lignosulfonate fully dispersed in the acidic aqueous solution to obtain wood Sodium Sulfonate Solution.

[0031] (2) Treat the sodium lignosulfonate solution with 150W and 40kHz ultrasonic waves at 25°C for 60 minutes. The ultrasonic reaction solution is naturally cooled, then the solvent is removed by distillation under reduced pressure and dried at a constant temperature to obtain a dark brown ultrasonic sample of sodium lignosulfonate. The content of phenolic hydroxyl group was used as the standard, and the measurement was carried out according to ultraviolet differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1): 213-221.). The phenolic hydroxyl content of lignosulfonate before ultrasound was 0.6553%, and the phenolic hydroxyl content of lignosulfonate after ultrasound wa...

Embodiment 2

[0036] (1) Dissolve 10g of sodium lignosulfonate in 100ml of distilled water, then adjust the pH to 2 with a 98% mass percent concentrated sulfuric acid solution, stir to make the sodium lignosulfonate fully dispersed in the acidic aqueous solution to obtain wood Sodium Sulfonate Solution.

[0037] (2) Treat the sodium lignosulfonate solution with 150W, 40kHz ultrasonic at 25°C for 60min. The ultrasonic reaction solution is naturally cooled, then the solvent is removed by vacuum distillation and dried at a constant temperature to obtain a dark brown ultrasonic sodium lignosulfonate sample. The content of phenolic hydroxyl group was used as the standard, and the measurement was carried out according to ultraviolet differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1): 213-221.). After ultrasound, the phenolic hydroxyl content of lignosulfonate increased from 0.6553% to 1.5539%, and the ultrasound efficiency reached 137%.

Embodiment 3

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

[0043] (2) Treat the sodium lignosulfonate solution with 150W, 40kHz ultrasonic at 30°C for 60min. The ultrasonic reaction solution is naturally cooled, and then the solvent is removed by vacuum distillation and dried at a constant temperature to obtain a dark brown sodium lignosulfonate sample. Taking the content of phenolic hydroxyl group as the standard, the content of phenolic hydroxyl group of lignosulfonate was increased from 0.6553% to 0.9166% after ultrasonic measurement by UV differential spectroscopy (Arthur Wexler S. Analytical Chemistry, 1964, 36(1): 213~221.) , The ultrasound 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 reaction activity of lignosulfonate, and particularly relates to a method and application for increasing the phenolic hydroxyl content of lignosulfonate by using ultrasonic waves. Background technique [0002] Lignosulfonates are derivatives of lignin, the second most abundant biomass resource in nature. The three-dimensional network of natural macromolecules is rich in nature and can be bio-renewable. As the largest source of natural aromatic compounds, it has many important uses, including as a phenol substitute to prepare phenolic resins, or modified to prepare natural surfactants and metal ion adsorbents. As the main waste and pollutant of the acidic paper pulping industry, lignosulfonate is inexpensive and has sufficient supply. Therefore, broadening its utilization range and improving its utilization value are of great significance to solving environmental pollution and protecting the ecological en...

Claims

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Application Information

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Patent Type & Authority Patents(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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