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Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid

A technology of ionic liquid and lignin, which is applied in the field of adhesives, can solve the problems of high energy consumption, large steric hindrance of substituents, and difficult operation, and achieve the effects of reducing the liquefaction residue rate, less corrosive equipment, and mild liquefaction conditions

Inactive Publication Date: 2012-06-13
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The molecular structure of natural lignin is complex, the molecular weight is high, and the substituents of the aromatic ring of lignin itself are relatively hindered, so it cannot react effectively with phenolic resin
This problem can be improved by modifying lignin, but the modified lignin adhesive still has problems: high molecular weight and high viscosity, which affect the wide application of lignin adhesive
The high-temperature and high-pressure liquefaction method needs to be carried out under high temperature and high pressure, which is not easy to operate and consumes a lot of energy; the low-temperature liquefaction method requires the use of acidic or alkaline catalysts, which is corrosive to equipment and seriously pollutes the environment

Method used

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  • Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid
  • Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid
  • Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 10g[bmin]Cl and 0.5g straw into a three-neck flask, 2 Heat to 100 DEG C in a stirring oil bath, react for a period of time, when the color of the solution turns purple brown from colorless, stop the reaction, add 0.5g formaldehyde and 3g sodium hydroxide (adding with 30% concentration) after cooling, Under normal pressure, raise the temperature to 40°C and react for 5 minutes, then raise the temperature to 80°C and react for 3 hours, measure the viscosity (viscosity is controlled at about 3-6s) by the reverse bubble method, and stop heating when it meets the adhesive requirements to obtain the adhesive.

Embodiment 2

[0030] 5g 3,3'-ethyl-1,2-bis(N-methylimidazolium) chloride salt and 0.5g straw were added in the three-necked flask, under N 2 Heat to 80 ℃ in a stirring oil bath, react for a period of time, when the color of the solution changes from colorless to purple brown, stop the reaction, add 1.5g formaldehyde and 2g sodium hydroxide (adding with 40% concentration) after cooling, Under normal pressure, raise the temperature to 50°C and react for 10 minutes, then raise the temperature to 90°C and react for 2 hours, measure the viscosity (viscosity is controlled at about 3-6s) by the reverse bubble method, and stop heating when it meets the adhesive requirements to obtain the adhesive.

Embodiment 3

[0032] Add 10g NMPCl and 0.5g straw into the three-neck flask, 2 Heat to 120 DEG C in a stirring oil bath, react for a period of time, when the color of the solution turns purple-brown from colorless, stop the reaction, add 0.5g formaldehyde and 3g sodium hydroxide (adding with 30% concentration) after cooling, in Under normal pressure, raise the temperature to 40°C and react for 5 minutes, then raise the temperature to 80°C and react for 3 hours, measure the viscosity (viscosity is controlled at about 3-6s) by the reverse bubble method, and stop heating when it meets the adhesive requirements to obtain the adhesive.

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Abstract

The invention relates to a method of preparing phenolic resin through liquefaction of lignin by using ionic liquid. The invention is characterized in that ionic liquid which comprises mono-core or double-core nitrogen-containing cations of alkyl imidazole, alkyl pyridine, quaternary ammonium salt and the like and anions and is in a liquid state at room temperature is used as a liquefaction reagent to liquefy lignin and a product of liquefaction is used to prepare the phenolic resin. Compared to the traditional phenol / sulfuric acid method, the liquefaction method provided in the invention has the characteristics of simple flow, a high liquefaction ratio, low corrosivity, clean process, capacity of adjusting the structure of the liquefaction reagent, repeatedly using the liquefaction reagent and facilitating environmental protection, etc.; the phenolic resin prepared from lignin does not contain volatile phenol, thereby reducing release amount of formaldehyde and being energy saving and environment friendly.

Description

technical field [0001] The invention belongs to the technical field of adhesives, and in particular relates to a method for preparing phenolic adhesives by using ionic liquid to liquefy lignin. Background technique [0002] With the requirements of sustainable development and the enhancement of people's awareness of environmental protection, the research and development of biodegradable environment-friendly products has attracted more and more international attention and attention. Among the phenolic resins, the phenolic resin formed by the polycondensation of phenol and formaldehyde is the most widely used, and its glued products have strong bonding strength, water resistance, heat resistance, and corrosion resistance. However, phenolic resin has high hot-pressing temperature and time. Shortcomings such as long and short, are subject to certain restrictions in use, and because phenol is a petrochemical product, the price of phenolic resin adhesive is relatively high. Ligni...

Claims

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Application Information

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IPC IPC(8): C09J161/06C08G8/08C08H8/00
Inventor 王海军季文艳施金才夏晓莉宋启霞许冰冰张华马洁丁振东
Owner JIANGNAN UNIV
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