Method for preparing highly sulfonated sodium lignosulfonate

A technology of sodium lignosulfonate and high sulfonation degree, applied in the directions of lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of harsh reaction conditions, limiting the industrial application of alkali lignin sulfonation modification, etc. , to achieve the effect of easy process control, improved utilization value and high efficiency

Inactive Publication Date: 2009-07-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Harsh reaction conditions limit the industrial application of alkali lignin sulfonation modification

Method used

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  • Method for preparing highly sulfonated sodium lignosulfonate

Examples

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Embodiment 1

[0025] Take 100g of wheatgrass alkali lignin, add 300g of distilled water, stir for 30 minutes, adjust the pH value of the solution to 3 with dilute sulfuric acid (10% Wt), and filter. Add 400g of 2.5wt% NaOH solution to the precipitate, heat to 50°C while stirring, dropwise add 50g of aqueous solution containing 5g of ammonium persulfate and 2g of ferrous sulfate, and slowly heat up to 65°C for free radical degradation reaction, and react for 10 minutes ; Under the state of stirring, drop 7g paraformaldehyde (polymerization degree 8~100, Shanghai Huishen Chemical Co., Ltd.), after fully stirring evenly, be placed in the frequency conversion microwave reactor, adjust the power to be 300W, control the temperature to be 70 °C, after reacting for 10 minutes, 50 g of an aqueous solution containing 20 g of sodium sulfite was added. The mixture was placed in a microwave reactor, the power was adjusted to 300W, the temperature was controlled to 85°C, and the reaction was carried out ...

Embodiment 2

[0027] Take 100g of wheatgrass alkali lignin, add 300g of distilled water, stir for 30 minutes, adjust the pH value of the solution to 3 with dilute sulfuric acid (10% Wt), and filter. Add 400g of 2.5wt% NaOH solution to the precipitate, heat to 50°C while stirring, add dropwise 50g of an aqueous solution containing 30g of ammonium persulfate and 5g of ferrous sulfate, and slowly heat up to 75°C for free radical degradation reaction, and keep warm for 30 minutes ; In the state of stirring, drop 12g paraformaldehyde (polymerization degree 8~100, Shanghai Huishen Chemical Co., Ltd.), after fully stirring evenly, place in the frequency conversion microwave reactor, adjust the power to be 300W, and control the temperature to be 85 After reacting for 15 minutes, 50 g of an aqueous solution containing 50 g of sodium sulfite was added. The mixture was placed in a microwave reactor, the power was adjusted to 800W, the temperature was controlled to 95°C, and the reaction was carried ou...

Embodiment 3

[0029] Take 100g of wheatgrass alkali lignin, add 300g of distilled water, stir for 30 minutes, adjust the pH value of the solution to 3 with dilute sulfuric acid (10% Wt), and filter. Add 400g of 2.5wt% NaOH solution to the precipitate, heat to 50°C while stirring, dropwise add 50g of an aqueous solution of 25g ammonium persulfate and 4g ferrous sulfate, and slowly heat up to 75°C for free radical degradation reaction, and keep warm for 50 minutes; In the state of stirring, add 15g of paraformaldehyde (polymerization degree 8-100, Shanghai Huishen Chemical Co., Ltd.) dropwise, after fully stirring evenly, place it in a frequency conversion microwave reactor, adjust the power to 300W, and control the temperature to 75°C After 10 minutes of reaction, 50 g of aqueous solution containing 40 g of sodium sulfite was added. The mixture was placed in a microwave reactor, the power was adjusted to 1000W, the temperature was controlled to 85°C, and the reaction was carried out for 2.0 ...

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Abstract

The invention discloses a method for preparing sodium lignin sulfonate with high sulfonation degree. A side product, namely wheat straw alkali lignin of a paper-making waste liquid is taken as a main raw material for a free radical degradation reaction under water bath heating conditions under normal pressure at a temperature of between 65 and 75 DEG C, and then an aldehyde substance is dripped to react for 10 to 20 minutes under microwave radiation conditions; and then 50 weight portions of aqueous solution containing 20 to 50 weight portions of sulfonating agent is added into the mixture to react for 1.0 to 2.5 hours under microwave power of between 300 and 1,200W to prepare the sodium lignin sulfonate with higher sulfonation degree. Compared with the prior alkali lignin sulfonation reaction, the technology prepares the sodium lignin sulfonate with high sulfonation degree and water solubility by initiating the degradation of free radicals of lignin, synergistically coordinating microwave radiation effect, using paraformaldehyde to increase active hydroxyl groups in the lignin, increasing the length of an alkyl chain, and then performing a sulfonation reaction, and the sulfonation degree of the sodium lignin sulfonate is higher than 3mmol/g.

Description

technical field [0001] The invention relates to the preparation of sodium lignosulfonate, in particular to a preparation method of sodium lignosulfonate with high sulfonation degree. Background technique [0002] A large amount of waste liquid is produced in the paper pulping process, and lignosulfonate and alkali lignin are the main components of acid pulping and alkaline process wastewater, respectively. Because of its surface activity, lignosulfonate can be recycled as oil field surfactants, concrete additives, agricultural chemicals, industrial adhesives, etc., while the dominant alkaline pulping produces a large amount of alkali lignin due to its application performance Poor, low chemical reactivity, lack of application pathways, usually under pressure from the environment, through combustion to utilize heat and recover alkali. Alkali recovery equipment requires a large investment and high operating costs. Small and medium-sized chemical pulp mills below 20,000 tons ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G1/00C02F9/04C02F103/28C08H7/00
Inventor 邱学青欧阳新平杨东杰柯丽瑄
Owner SOUTH CHINA UNIV OF TECH
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