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Synthesizing method of epoxy resin by autocatalysis of lignin

A technology of epoxy resin and lignin, which is applied in the field of lignin utilization, can solve the problems of high-boiling alcohol lignin extraction process complexity, low extraction rate, and high cost, so as to create economic value and social value, improve safety, reduce The effect of polluting emissions

Inactive Publication Date: 2012-09-19
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In previous studies, it was reported that lignosulfonate was modified or epoxy resin was synthesized from high-boiling alcohol lignin, but lignosulfonate had a high ash content and poor activity, and the modification used The substance has certain toxicity; while the extraction process of high boiling alcohol lignin is complex, the extraction rate is low, and the cost is high, and the time required for the preparation of epoxy resin is longer

Method used

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  • Synthesizing method of epoxy resin by autocatalysis of lignin

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Effect test

Embodiment 1

[0011] Utilize 20% mass fraction of sulfuric acid solution to adjust the pH of papermaking black liquor to 8.5, filter to remove ash and impurities, and obtain lignin alkali solution; weigh 5.13g of bisphenol A, place it in a 250mL three-necked flask, and transfer it into a 19.6mL ring Oxychloropropane, stirred in a water bath at 50°C until fully dissolved; add 1mL lignin alkali solution to the system as a catalyst, react for 30min, heat up to 90°C, then add 21mL lignin alkali solution to the solution, lignin The addition ratio is equivalent to 10wt.%, and the stirring is stopped after 1 hour of reaction; the product is filtered hot, and the filtrate is collected for vacuum distillation to remove residual moisture and excess epichlorohydrin. Finally, epoxy resin was obtained, which was a brown viscous liquid, and the yield and epoxy value were shown in Table 1.

Embodiment 2

[0013] Utilize 20% mass fraction of sulfuric acid solution to adjust the pH of papermaking black liquor to 8.5, filter to remove ash and impurities, and obtain lignin alkali solution; weigh 4.85g of bisphenol A, place it in a 250mL three-necked flask, and transfer it into a 19.6mL ring Oxychloropropane, stirred in a water bath at 50°C until fully dissolved; add 1mL lignin alkali solution to the system as a catalyst, react for 30min, heat up to 90°C, then add 32mL lignin alkali solution to the solution, lignin The addition ratio is equivalent to 15wt.%, and the stirring is stopped after 1 hour of reaction; the product is filtered hot, and the filtrate is collected for vacuum distillation to remove residual water and excess epichlorohydrin. Finally, epoxy resin was obtained, which was a brown viscous liquid, and the yield and epoxy value were shown in Table 1.

Embodiment 3

[0015] Utilize 20% mass fraction of sulfuric acid solution to adjust the pH of papermaking black liquor to 8.5, filter to remove ash and impurities, and obtain lignin alkali solution; weigh 4.56g of bisphenol A, place it in a 250mL three-necked flask, and transfer it into a 19.6mL ring Oxychloropropane, stirred at 50°C water bath temperature until fully dissolved; add 1mL lignin alkali solution to the system as a catalyst, react for 30min, heat up to 90°C, then add 43mL lignin alkali solution to the solution, lignin The addition ratio is equivalent to 20wt.%, and the stirring is stopped after 1 hour of reaction; the product is filtered hot, and the filtrate is collected for vacuum distillation to remove residual moisture and excess epichlorohydrin. Finally, epoxy resin was obtained, which was a brown viscous liquid, and the yield and epoxy value were shown in Table 1.

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Abstract

The invention relates to a method for preparing bisphenol-A epoxy resin partially substituted with lignin in a normal-pressure low-temperature water-bath condition through autocatalysis of lignin from papermaking black liquor.. The method comprises the following steps: removing impurities of the papermaking black liquor through acid out; filtering to obtain a lignin alkaline solution; mixing bisphenol-A, epichlorohydrin and the lignin alkaline solution, and sufficiently reacting in a heating and stirring condition by utilizing the autocatalytic effect of the lignin alkaline solution; filtering the product, and distilling the filtrate under reduced pressure to obtain epoxy resin brown viscous liquid finally. The method has the advantages that discharge of papermaking black liquor is reduced, waste utilization is realized, the nontoxic and harmless lignin is utilized as the raw material, and safety of the epoxy resin is improved; reaction conditions are mild, other catalysts or modifying agents are not added, the operation process, is simple, the effects of energy saving and cost reduction are achieved, and economical and social value are created; therefore the method has very important practical significance.

Description

technical field [0001] The present invention relates to a new method for utilizing lignin in papermaking black liquor, in particular to using lignin in papermaking black liquor as a raw material, and autocatalytically preparing lignin to partially replace bisphenol A epoxy resin under normal pressure and low temperature conditions new method. Background technique [0002] Epoxy resin generally refers to organic polymer compounds containing two or more epoxy groups in the molecule. The biggest feature of epoxy resin is that the molecular chain contains active epoxy groups, and the epoxy groups can be located in the molecule. The middle, terminal or cyclic structure of the chain, its relative molecular weight generally belongs to the range of oligomers. Epoxy resin has been widely used both in daily life and in cutting-edge technology fields due to its excellent bonding properties, mechanical properties, and electrical properties. [0003] At present, most epoxy resins are p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
Inventor 田玉美张健王子忱王晓峰邹博朱燕超
Owner JILIN UNIV
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