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Lignin-based polyol for synthesizing polyurethane and preparation method of lignin-based polyol

A technology based on lignin and polyurethane, which is applied in the field of lignin modification, can solve the problems of large alkali consumption, affecting compatibility, and long degradation reaction time, and achieves less inorganic ash, good compatibility, and structural change little effect

Active Publication Date: 2021-05-11
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is: lignin may be accompanied by side reactions such as crosslinking during the reaction process, which will affect the compatibility of lignin with other components of synthetic polyurethane
However, due to the large amount of alkali consumption in the lignin depolymerization process, according to Example 1, the amount of sodium hydroxide is as high as 80% of the lignin quality, and the degradation reaction time is as long as 8 hours; in addition, the hydroxyl content of lignin after depolymerization Only increased by about 0.4mmol / g than before the reaction

Method used

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  • Lignin-based polyol for synthesizing polyurethane and preparation method of lignin-based polyol

Examples

Experimental program
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Effect test

Embodiment 1

[0040] (1) Hydrothermal degradation of lignin: Dissolve 10g of lignin acetate in 500mL of sodium hydroxide aqueous solution (concentration: 0.5mol / L) to obtain a mixed solution, and add 0.5g of manganese dioxide as a catalyst at the same time, and heat up after uniform mixing React at 200°C for 60 minutes; after the reaction is completed and cool to room temperature, filter the insoluble matter with a Buchner funnel to obtain the filtrate, then adjust the pH value of the filtrate to 2.0-3.0 with dilute HCl solution to precipitate precipitates; filter and wash the precipitates repeatedly with deionized water , until the pH of the filtrate from the last wash is close to neutral, and finally placed in a vacuum oven at 50° C. for 24 hours, and ground to obtain degraded lignin. The number-average molecular mass of the degraded lignin measured by gel chromatography was 2052, and the hydroxyl content was 7.06mmol / g.

[0041] (2) Hydroxylation modification of degraded lignin: Weigh 10...

Embodiment 2

[0046] (1) Hydrothermal degradation of lignin: Dissolve 10g lignin acetate in 100mL sodium hydroxide aqueous solution (0.4mol / L) to obtain a mixed solution, add 0.5g manganese dioxide as a catalyst, and heat up to React at 150°C for 30 minutes, after the reaction is completed and cool to room temperature, filter the insoluble matter with a Buchner funnel to obtain the filtrate, then adjust the pH value of the filtrate to 2.0-3.0 with dilute HCl solution to precipitate precipitates; the precipitates are repeatedly filtered and washed with deionized water, Until the pH of the filtrate from the last wash is close to neutral, it is finally placed in a vacuum oven at 50°C for 24 hours, and ground to obtain degraded lignin. The number-average molecular weight of the degraded lignin is 3056, and the hydroxyl content is 5.21mmol / g.

[0047] (2) Hydroxylation modification of degraded lignin: the method is the same as in Example 1 to obtain the lignin-based polyol for synthesizing polyu...

Embodiment 3

[0049] (1) Hydrothermal degradation of lignin: Dissolve 10g lignin acetate in 500mL sodium hydroxide aqueous solution (0.4mol / L) to obtain a mixed solution, add 0.5g manganese dioxide as a catalyst, and heat up to React at 150°C for 30 minutes, after the reaction is completed and cool to room temperature, filter the insoluble matter with a Buchner funnel to obtain the filtrate, then adjust the pH value of the filtrate to 2.0-3.0 with dilute HCl solution to precipitate precipitates; the precipitates are repeatedly filtered and washed with deionized water, Until the pH of the filtrate from the last wash is close to neutral, it is finally placed in a vacuum oven at 50°C for 24 hours, and ground to obtain degraded lignin. The number-average molecular mass of the degraded lignin is 2905, and the hydroxyl content is 5.41mmol / g.

[0050] (2) Hydroxylation modification of degraded lignin: the method is the same as in Example 1 to obtain the lignin-based polyol for synthesizing polyure...

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Abstract

The invention belongs to the technical field of polyurethane synthesis, and discloses lignin-based polyol for synthesizing polyurethane and a preparation method of the lignin-based polyol. The method comprises the following steps: carrying out hydrothermal degradation on acetic acid lignin under the catalysis of a metal oxide, and precipitating a degradation product with dilute acid; and carrying out hydroxylation modification on the degraded lignin to obtain the polyhydroxy lignin polyol. The method provided by the invention solves the problems of low lignin reaction activity, low reaction participation degree, poor compatibility of lignin and a polyurethane matrix and the like. The required lignin raw material is wide in source, environment-friendly and degradable, and high-value utilization of the lignin is realized. In the preparation method provided by the invention, the adopted raw material acetic acid lignin has good solubility in an organic solvent, contains less inorganic matter ash, has less structural change, and is beneficial to subsequent structural modification and application.

Description

technical field [0001] The invention belongs to the technical field of lignin modification, and in particular relates to a lignin-based polyol used for synthesizing polyurethane and a preparation method thereof. Background technique [0002] Polyurethane is generally a polymer with repeating structural units of urethane chain segments made by the reaction of dibasic or polybasic organic isocyanates and polyol compounds. At present, the raw materials for the production of polyurethane mainly come from petrochemical products. Due to the depletion of petroleum resources, raw materials derived from petroleum are also facing shortages. The extensive use of petrochemical resources has also caused serious environmental problems. Traditional polyurethane is difficult to degrade and recycle, causing certain pollution to the environment. Currently, attempts are being made to replace petrochemicals with renewable biomass feedstocks for the production of polyol components for the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08G18/64
CPCC08H6/00C08G18/6492
Inventor 何甜谌凡更马榆羊董昕宇朱文祥
Owner SOUTH CHINA UNIV OF TECH
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