Demethylated lignin liquid modified phenolic resin as well as preparation method and application thereof in phenolic foam

A demethylation and phenolic resin technology, applied in the field of thermal insulation materials, can solve the problems of high price of cetyl tri-n-butylphosphorus bromide and difficulty in industrial application, and achieve reduction of reaction activation energy, strong mechanical properties, The effect of low free formaldehyde content

Active Publication Date: 2020-07-10
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The price of hexadecyl tri-n-butylphosphorus bromide used in the modification is relatively high, and the modification needs to be carried out in DMF, which is difficult for industrial application

Method used

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  • Demethylated lignin liquid modified phenolic resin as well as preparation method and application thereof in phenolic foam
  • Demethylated lignin liquid modified phenolic resin as well as preparation method and application thereof in phenolic foam
  • Demethylated lignin liquid modified phenolic resin as well as preparation method and application thereof in phenolic foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Take 100 parts of phenol, add 20 parts of lignin, add 8 parts of hydrobromic acid aqueous solution with a mass fraction of 48%, put the mixture in an atmospheric pressure microwave reactor at 80°C for 2 hours, and cool to 50°C to obtain Methylated lignin liquid; add 30wt% sodium hydroxide aqueous solution to the above-mentioned demethylated lignin liquid, adjust the pH to 8.5-9.0; take 100 parts of phenol, add 45 parts of paraformaldehyde in two batches, 8 parts of basic catalyst (sodium hydroxide) and 35 parts of water, add 50% by mass fraction of paraformaldehyde, 50% by mass fraction of basic catalyst and 50% by mass of water for the first time, heat up to 80°C and react for 1h , add the remaining paraformaldehyde, basic catalyst and water to the reaction solution again, react at 80°C for 0.5h, and cool down to 65°C to obtain the demethylated lignin liquid modified phenolic resin; the phenolic resin The pH value is 8.4, the solid content is 76wt%, the viscosity is 29...

Embodiment 2

[0054] Take 100 parts of phenol, add 30 parts of lignin, add 7 parts of hydrobromic acid aqueous solution with a mass fraction of 48%, put the mixture in an atmospheric pressure microwave reactor at 90°C for 2 hours, and cool to 50°C to obtain the Methylated lignin liquid; add 30wt% sodium hydroxide aqueous solution to the above-mentioned demethylated lignin liquid, adjust the pH to 8.5-9.0; take 100 parts of phenol, add 42 parts of paraformaldehyde in two batches, 8.5 parts of basic catalyst (sodium hydroxide) and 40 parts of water, add 50% by mass fraction of paraformaldehyde, 50% by mass fraction of basic catalyst and 50% by mass of water for the first time, heat up to 90°C and react for 1h , add the remaining paraformaldehyde, basic catalyst and water to the reaction solution again, react at 90°C for 0.5h, and cool down to 65°C to obtain the demethylated lignin liquid modified phenolic resin; the phenolic resin The pH value is 8.5, the solid content is 78wt%, the viscosity...

Embodiment 3

[0057] Take 100 parts of phenol, add 40 parts of lignin, add 6 parts of hydrobromic acid aqueous solution with a mass fraction of 48%, put the mixture in an atmospheric pressure microwave reactor at 100°C for 1.5h, and cool to 50°C to obtain Demethylated lignin liquid; add 30wt% sodium hydroxide aqueous solution to the above demethylated lignin liquid, adjust the pH to 8.5-9.0; add 38 parts of paraformaldehyde in two batches based on 100 parts of phenol , 9 parts of basic catalyst (sodium hydroxide) and 42 parts of water, add the water of the paraformaldehyde of 50% mass fraction, the basic catalyst of 50% mass fraction and 50% mass fraction for the first time, be warming up to 85 ℃ of reaction 1h, add the remaining paraformaldehyde, basic catalyst and water to the reaction solution again, react at 85°C for 0.5h, and cool down to 65°C to obtain the demethylated lignin liquid modified phenolic resin; the phenolic resin The pH value is 8.6, the solid content is 80wt%, the viscos...

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Abstract

The invention discloses demethylated lignin liquid modified phenolic resin as well as a preparation method and application thereof in phenolic foam. The pH value of the modified phenolic resin is 8.3-8.6, the solid content is 75%-80%, the viscosity is 1800-4000cp, and the gelation time is 80-100 seconds. The method has the following advantages that: (1) microwave assistance is adopted, the ligninis demethylated by using haloid acid, the reaction sites of the demethylated lignin are increased, and the solvent used for lignin modification is phenol, so that the demethylated lignin liquid does not need to be further treated and can directly replace phenol to prepare phenolic resin and phenolic foam, and therefore, the production process of the resin and foam is simplified; and (2) compared with unmodified lignin-based phenolic foam, the phenolic foam prepared by the method in the invention has lower heat conductivity coefficient, stronger mechanical property and higher oxygen index, andhas a market application prospect.

Description

technical field [0001] The invention belongs to the field of thermal insulation materials, and in particular relates to a demethylated lignin liquid modified phenolic resin, a preparation method thereof and an application in phenolic foam. Background technique [0002] Phenolic foam is a thermosetting rigid foam made of phenolic resin as the main raw material, cross-linked, foamed and cured with the participation of foaming agent, surfactant, curing agent and other additives. Due to its unique advantages such as excellent flame retardancy, thermal stability, heat insulation, low combustion toxicity, corrosion resistance, high modulus, etc., phenolic foam is widely used in construction, petrochemical, vehicle and ship, aerospace industry and other fields. It has been widely used, and it is known as the "King of Thermal Insulation" because of its own performance characteristics. [0003] Lignin is an aromatic polymer with a three-dimensional network structure formed by three ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/20C08H7/00C08L61/12C08L83/04C08L71/02C08K3/22C08J9/14
CPCC08G8/20C08H6/00C08J9/0061C08J9/0066C08J9/141C08J2203/14C08J2361/12C08J2471/02C08J2483/04C08K2003/2227
Inventor 朱晨杰胡有钦李明应汉杰庄伟高成陈勇柳东牛欢青杨朋朋
Owner NANJING TECH UNIV
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