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In-situ ultrasonic polymerization preparation method for industrial alkali lignin modified phenolic resin

A technology of industrial alkali lignin and phenolic resin, which is used in the joining of wooden veneers, aldehyde/ketone condensation polymer adhesives, manufacturing tools, etc. The effect of simple control and preparation process

Active Publication Date: 2014-01-08
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using papermaking waste industrial alkali lignin as raw material to replace part of phenol, the method of in-situ ultrasonic polymerization was used to prepare lignin phenolic resin, which solved the problems of repolymerization and activity reduction after lignin was degraded by simple ultrasonic treatment. Lignin-modified phenolic resin with high phenol substitution

Method used

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  • In-situ ultrasonic polymerization preparation method for industrial alkali lignin modified phenolic resin
  • In-situ ultrasonic polymerization preparation method for industrial alkali lignin modified phenolic resin
  • In-situ ultrasonic polymerization preparation method for industrial alkali lignin modified phenolic resin

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 500g of wheatgrass alkali lignin powder into a beaker, add 4500g of water, adjust the pH to 12 with 10% sodium hydroxide solution, and centrifuge to get the supernatant. Then add sulfuric acid solution with a mass concentration of 10% to adjust the pH value to 2, react at 75° C. for 30 minutes, centrifuge, and the precipitate is vacuum-dried to constant weight after repeated washing to obtain purified alkali lignin.

[0023] Weigh 20g of purified alkali lignin, 80g of phenol, 32g of formaldehyde solution with a mass concentration of 37%, and 129g of NaOH solution with a mass concentration of 20%. The power is 600W, and the ultrasonic time is 10min; transfer the reaction solution into a 500ml four-necked flask, start stirring, and heat up to 85°C within 45min, and react for 17min; cool the reaction solution below 50°C, and add 135g of 37% For formaldehyde solution, heat up to 85°C within 50 minutes, and react for 15 minutes; cool the reaction solution to 70°C, reac...

Embodiment 2

[0025] Weigh 500g of wheatgrass alkali lignin powder into a beaker, add 4500g of water, adjust the pH to 12 with 10% sodium hydroxide solution, and centrifuge to get the supernatant. Then add sulfuric acid solution with a mass concentration of 10% to adjust the pH value to 2, react at 75° C. for 30 minutes, centrifuge, and the precipitate is vacuum-dried to constant weight after repeated washing to obtain purified alkali lignin.

[0026] Weigh 20g of purified alkali lignin, 80g of phenol, 32g of formaldehyde solution with a mass concentration of 37%, and 129g of NaOH solution with a mass concentration of 20%. The power is 750W, and the ultrasonic time is 10min; transfer the reaction solution into a 500ml four-neck flask, start stirring, and heat up to 85°C within 45min, and react for 17min; cool the reaction solution below 50°C, and add 135g of 37% For formaldehyde solution, heat up to 85°C within 50 minutes, and react for 15 minutes; cool the reaction solution to 70°C, react ...

Embodiment 3

[0028] Weigh 500g of wheatgrass alkali lignin powder into a beaker, add 4500g of water, adjust the pH to 12 with 10% sodium hydroxide solution, and centrifuge to get the supernatant. Then add sulfuric acid solution with a mass concentration of 10% to adjust the pH value to 2, react at 75° C. for 30 minutes, centrifuge, wash the precipitate with water, and then vacuum-dry to constant weight to obtain purified alkali lignin.

[0029] Weigh 20g of purified alkali lignin, 80g of phenol, 32g of formaldehyde solution with a mass concentration of 37%, and 129g of NaOH solution with a mass concentration of 20%. The power is 900W, and the ultrasonic time is 10min; transfer the reaction solution into a 500ml four-necked flask, start stirring, and heat up to 85°C within 45min, and react for 17min; cool the reaction solution below 50°C, and add 135g of 37% For formaldehyde solution, heat up to 85°C within 50 minutes, and react for 15 minutes; cool the reaction solution to 70°C, react for ...

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Abstract

The invention relates to an in-situ ultrasonic polymerization preparation method for industrial alkali lignin modified phenolic resin. The in-situ ultrasonic polymerization preparation method comprises the following steps of performing alkali dissolution, acid precipitation, centrifugation, washing and drying on 5-10% by mass of industrial alkali lignin liquor to obtain purified alkali lignin; successively adding the lignin, part of formaldehyde solution, phenol and alkali in an in-situ ultrasonic reactor, and performing high-energy ultrasonic irradiation treatment on the mixture; and performing further polymerization reaction by adding the rest formaldehyde and alkali in a product obtained after treatment, and carrying out heating, heat preservation and cooling on the product to obtain the lignin modified phenolic resin. The in-situ ultrasonic polymerization preparation method is characterized in that lignin macromolecular structures are damaged by using multiple actions such as breakage, activation and triggering which are generated by ultrasonic waves, and a phenol type structure containing vacancy is formed, and is then triggered to be added with formaldehyde, so that high-performance resin with high phenol substitution is obtained. The in-situ ultrasonic polymerization preparation method solves the problems that the existing pure lignin is easy to polymerize and the activity of the existing pure lignin is reduced after the existing pure lignin is degraded under the action of ultrasonic cavitation.

Description

technical field [0001] The invention belongs to the field of wood adhesives, and in particular relates to a method for preparing lignin-modified phenolic resin from alkali lignin in the papermaking industry. Background technique [0002] Phenolic resin adhesive has excellent bonding strength, water resistance and heat resistance, and is widely used in the production of outdoor wood products. However, its main raw material, phenol, is a petrochemical product. With the shortage of petroleum resources, the price continues to rise, and it has a large toxicity. Therefore, the use of renewable resources instead of phenol to prepare phenolic resin adhesives is the focus of current research. [0003] Lignin is a natural organic macromolecular substance synthesized by secondary metabolism of plants. It has aldehyde groups and phenol structural units and can be used in the preparation of phenolic resins. As a big paper-making country, my country produces a large amount of paper-maki...

Claims

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Application Information

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IPC IPC(8): C08G8/28C09J161/14C09J103/02B27D1/04
Inventor 连海兰程明娟潘明珠周晓燕梅长彤黄润洲杨蕊洪枢孙香潘栋姜彬
Owner NANJING FORESTRY UNIV
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