Hot melt type phenolic resin modified by using enzymatic hydrolysis lignin or derivatives thereof, and preparation thereof

A technology for enzymatic hydrolysis of lignin and phenolic resin is applied in the field of polymer thermoplastic material preparation to achieve the effects of low manufacturing cost, improved performance and reduced dosage

Active Publication Date: 2009-04-22
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of enzymolysis lignin or its derivative modified hot-melt phenolic resin and preparation method; The existing technology extracts the defects caused by lignosulfonate from the "black liqu

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045]First heat and melt phenol (crystallization at room temperature), add 94 grams of phenol into the three-necked flask, then add 19 grams of enzymatic lignin and 1 gram of p-toluenesulfonic acid catalyst, heat to 80 ° C and stir to dissolve the lignin and catalyst in the phenol After completely dissolving, continue heating and stirring for 0.5h, then dropwise add 81 grams of formaldehyde with a concentration of 37%, heat to maintain the polycondensation reaction at about 85-90°C, and start dehydration under reduced pressure to remove small molecular substances such as water after reacting for 2 hours. The decompression conditions are 480-500mmHg, 110°C, 2 hours, and finally the resin is heated to 125-130°C and poured out to obtain 118 grams of enzymatic lignin modified thermoplastic phenolic resin. The resin is black in color, brown in powder form, and has a melting point of 94°C.

Embodiment 2

[0047] Heat and melt phenol (crystallization at room temperature), add 94 grams of phenol into a three-necked flask, then add 14 grams of enzymatic lignin and 1.2 grams of oxalic acid catalyst, heat to 80 ° C and stir to dissolve lignin and catalyst in phenol and dissolve completely Then continue heating and stirring for 0.5h, then dropwise add 81 grams of formaldehyde with a concentration of 37%, and heat to keep the polycondensation reaction at about 85-90°C. After reacting for 2 hours, start dehydration under reduced pressure to remove small molecules such as water. The reduced pressure condition is 480-500mmHg, 110°C, 2 hours, and finally heat the resin to 125-130°C and pour it out to obtain 110 grams of enzymatic lignin-modified thermoplastic phenolic resin. The resin is black in color, brown in powder form, and has a melting point of 96°C.

Embodiment 3

[0049] First, enzymatic lignin-maleic anhydride derivatives were prepared according to the following method: the enzymatic lignin was ground into 80-mesh powder, and vacuum-dried at 60°C. Take 100 grams of enzymatic lignin and 3 grams of maleic anhydride, and then add 0.5 grams of dicumyl peroxide (DCP) as an initiator for free radical polymerization. Put the mixture into an airtight mixer and stir at high speed to disperse and mix evenly. Then the mixture was put into a torque rheometer, and reacted for 10 minutes under the conditions of 140° C. and 50 r / min rotation speed. The resulting product was taken out and ground into a powder. Maleic anhydride is not easy to self-polymerize, and will only form a homopolymer composed of one or two monomers. They and unreacted maleic anhydride are both easily soluble in water, while enzymatic lignin is insoluble in water at low temperature. Therefore, for purification, the reaction product was soaked in water (4° C.) for 12 hours to ...

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Abstract

The invention provides enzymatic lignin or a derivative for the enzymatic lignin, namely modified hot-melt phenol-formaldehyde resin and a preparation method thereof, wherein the enzymatic lignin or the derivative for the enzymatic lignin, phenols, aldehydes and catalysts are taken as raw materials. The preparation method comprises the following steps: the enzymatic lignin or the derivative for the enzymatic lignin is mixed with the phenols according to the proportion; the mixture is heated and dissolved, added with the aldehydes and the catalysts, and subjected to heating and refluxing for a period of time; and residual water in the system is distilled, and the enzymatic lignin or the derivative for the enzymatic lignin, namely the modified hot-melt phenol-formaldehyde resin is obtained. The preparation method fully utilizes reproducible biological resources, overcomes the defects caused by extracting lignosulphonate from paper-making 'black liquor' in the prior art, can replace partial raw materials of the petrochemical industry, reduce the cost of preparing the phenol-formaldehyde resin by adopting phenyl hydroxide, select proper types of enzymatic lignin additives according to the modification requirements of different types of hot-melt phenol-formaldehyde resin, and improve the performance of the enzymatic lignin or the derivative for the enzymatic lignin, namely the modified hot-melt phenol-formaldehyde resin, has simple technology, is easy to implement, reduces the production cost, and improves the competitive power of products.

Description

technical field [0001] The invention belongs to the field of polymer thermoplastic material preparation, and more specifically relates to an enzymatically hydrolyzed lignin or its derivative modified hot-melt phenolic resin and a preparation method thereof. Background technique [0002] Phenolic resin is a commonly used polymer material, it has low cost, bulk density , good flame retardancy, good processability and other characteristics, it has been widely used in many industries. However, phenolic resin is synthesized from phenol and formaldehyde as the main raw materials. Phenol is a product of petrochemical or coal chemical industry. With the shortage of these mineral resources, the cost of raw materials is increasing day by day, and the traditional phenolic resin production faces difficulties in sustainable development. [0003] There have been reports on the modification of lignin extracted from papermaking black liquor to prepare phenolic resins. However, the structu...

Claims

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Application Information

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IPC IPC(8): C08G8/28
Inventor 程贤甦方润
Owner FUZHOU UNIV
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