Method for preparing lignin-based polyhydric alcohol and polyurethane from solid-super-acid-catalyzed lignin or sulfonated lignin

A technology of lignosulfonate and solid superacid, which is applied in the direction of chemical recycling, can solve the problems of high corrosion of equipment and restrictions on large-scale production, and achieve the effect of improving economic efficiency

Inactive Publication Date: 2016-03-16
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the inorganic acids and alkalis used in liquefaction have disadvantages such as neutralization after the reaction and high corrosion to equipment, which restrict large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add solid superacid SO in the three-necked flask (500ml) 4 2- / SnO 2 (mass fraction is 1%), glycerin, PEG-400 (the mass ratio of PEG-400 and glycerol is 1:1). The three-necked flask was connected with a condenser, a mechanical stirrer and a sealed sieve respectively. Place the connected device in an oil bath at a set temperature to preheat for 5 minutes, then add a set mass of industrial lignin (solid-to-liquid ratio 1:1) to start the reaction and time it. After reacting at 100°C for 2 hours, the three-neck flask was placed in cold water and cooled rapidly. The hydroxyl value of the obtained polyol was 527 mgKOH / g, and the acid value was 0.02 mgKOH / g.

Embodiment 2

[0024] Add solid superacid SO in the three-necked flask (500ml) 4 2- / ZrO 2 (mass fraction is 3%), glycerol, PEG-400 (the mass ratio of PEG-400 and glycerol is 4:1). The three-necked flask was connected with a condenser, a mechanical stirrer and a sealed sieve respectively. Place the connected device in an oil bath at a set temperature to preheat for 5 minutes, then add wheatgrass sodium lignosulfonate according to the solid-to-liquid ratio of 1:5, start the reaction and time it. After reacting at 140°C for 1 hour, the three-necked flask was placed in cold water and cooled rapidly. The hydroxyl value of the obtained polyol was 643 mgKOH / g, and the acid value was almost 0 mgKOH / g.

Embodiment 3

[0026] Add solid superacid SO in the three-necked flask (500ml) 4 2- / ZrO 2 (mass fraction is 5%), glycerol, PEG-400 (the mass ratio of PEG-400 and glycerin is 8:1). The three-necked flask was connected with a condenser, a mechanical stirrer and a sealed sieve respectively. Preheat the connected device in an oil bath at a set temperature for 5 minutes, then add wheatgrass sodium lignosulfonate according to the solid-to-liquid ratio of 1:10, start the reaction and time it. After reacting at 160° C. for 10 minutes, the three-neck flask was placed in cold water and cooled rapidly. The hydroxyl value of the obtained polyol was 417 mgKOH / g, and the acid value was 00.01 mgKOH / g.

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Abstract

The invention discloses a method for preparing lignin-based polyhydric alcohol and polyurethane from solid-super-acid-catalyzed lignin or sulfonated lignin. The method comprises: under the normal pressure, putting a certain amount of solid super acid, glycerin, and polyethylene glycol-400 (PFG-40) into a reactor, performing pre-heating at a certain temperature, adding industrial lignin or sulfonated lignin, or wheat straw lignin, and performing mechanical stirring and cooling; and adding a dioxane aqueous solution into the obtained product according to a certain solid-to-liquid ratio, fully dissolving the obtained mixture, and performing centrifugation, filtering, and rotary evaporation of the obtained filtrate. The obtained dioxane aqueous solution can be reused after purification, and the obtained lignin-based polyhydric alcohol is subjected to index measurement. The filtered residue is washed and centrifuged to recycle solid super-acid for reuse. Then, a material of lignin-based polyurethane is prepared by taking lignin-based polyhydric alcohol as a raw material and reacting the lignin-based polyhydric alcohol with isocyanate. According to the method, solid super-acid is firstly used for catalyzing transformation of industrial lignin or sulfonated lignin to prepare polyhydric alcohol and polyurethane foam (PUF).

Description

technical field [0001] The invention belongs to the technical field of directional conversion of lignin or lignosulfonate, through the method, industrial lignin or lignosulfonate can be directionally converted into lignin-based polyols, and then used to prepare polyurethane foam materials. The reaction process The solid acid catalyst and solvent can be recycled and utilized conveniently, which is beneficial to improving the economy of preparing lignin-based polyols and polyurethane materials from lignin or lignosulfonate. Background technique [0002] Lignin is an amorphous polymer that exists in most terrestrial plants. Lignin, cellulose and hemicellulose are the main components of the plant skeleton. Lignin acts as an adhesive in plants to bind components such as cellulose, hemicellulose, and inorganic salts (mainly silicate) together to form a solid plant skeleton structure. As one of the three major components of the plant skeleton, lignin is the second largest renewabl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08G18/64C08J9/14C08J9/08C08G101/00
CPCY02P20/584
Inventor 徐建曲永水罗皓李宏强
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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