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Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof

A technology of phenolizing lignin and resorcinol, which is applied in the field of preparation of lignin modified phenolic resin, can solve the problems of low foam strength, low lignin activity, high free formaldehyde of lignin phenolic resin, and achieve phenol replacement rate High, high mechanical strength, effect of promoting reaction

Active Publication Date: 2015-09-09
重庆集凯科技服务有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Technical problem to be solved In order to solve the shortcomings of low lignin activity, high free formaldehyde of the prepared lignin phenolic resin and low foam strength, the present invention provides a modification method of phenolized lignin modified resorcinol-phenol-formaldehyde resin , specifically degrade lignin by phenolization under alkaline conditions, and then react with paraformaldehyde for condensation polymerization

Method used

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  • Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof
  • Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof
  • Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof

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Embodiment 1

[0029] The first step, lignin phenolization degradation treatment: add 4 parts of enzymatic lignin, 34 parts of phenol, and 0.8 parts of 50% NaOH solution into the reactor, raise the temperature to 85°C, and react for 60 minutes; the second step, cool down to 75°C , add 32 parts of formaldehyde solution, carry out condensation polymerization reaction for 10 minutes; the third step, add 24 parts of paraformaldehyde in six times, add 0.8 parts of 50% NaOH solution in four times and react at 75°C for 60 minutes, wherein, the polyformaldehyde added each time The amount of formaldehyde is the same, and the amount of basic catalyst is also the same; in the fourth step, the temperature is lowered to 50° C., and 2 parts of resorcinol are added to react for 20 minutes. A resorcinol-phenol-formaldehyde resin modified by phenolized lignin is obtained.

[0030] See attached table 1 for the basic performance of the resin and the performance of its foam material.

Embodiment 2

[0032] The first step, lignin phenolization degradation treatment: add 20 parts of sodium lignosulfonate, 12 parts of phenol, and 5.6 parts of 50% NaOH solution into the reactor, raise the temperature to 100°C, and react for 240 minutes; the second step, cool down to 90 ℃, add 4 parts of formaldehyde solution, carry out condensation polymerization reaction for 40min; the third step, add 20 parts of paraformaldehyde in six times, add 2.4 parts of 50% NaOH solution in four times and react at 90℃ for 100min, wherein, each time adding more The amount of polyoxymethylene is the same, and the amount of basic catalyst is also the same; in the fourth step, the temperature is lowered to 60° C., and 8 parts of resorcinol are added to react for 100 minutes. A resorcinol-phenol-formaldehyde resin modified by phenolized lignin is obtained.

[0033] See attached table 1 for the basic performance of the resin and the performance of its foam material.

Embodiment 3

[0035] The first step, lignin phenolization degradation treatment: add 10 parts of calcium lignosulfonate, 24 parts of phenol, and 4.5 parts of 50% KOH solution into the reactor, raise the temperature to 90°C, and react for 180 minutes; the second step, cool down to 85 ℃, add 20 parts of formaldehyde solution, and carry out condensation polymerization for 30 minutes; the third step, add 16 parts of paraformaldehyde in six times, add 1.5 parts of 50% KOH in four times, and react at 90℃ for 70 minutes, wherein, the paraformaldehyde added each time The amount of formaldehyde is the same, and the amount of basic catalyst is also the same; in the fourth step, the temperature is lowered to 80° C., and 6 parts of resorcinol are added to react for 70 minutes. A resorcinol-phenol-formaldehyde resin modified by phenolized lignin is obtained.

[0036] See attached table 1 for the basic performance of the resin and the performance of its foam material.

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Abstract

The invention discloses modified expandable resorcinol-phenol-formaldehyde resin and a preparation method thereof. The preparation method comprises the following steps: adding lignin, phenol and a basic catalyst into a reactor for phenolate and degradation of lignin; adding a formaldehyde solution for condensation reaction with phenolated lignin and phenol; adding paraformaldehyde for further condensation reaction with the basic catalyst; adding resorcinol for condensation polymerization, so as to obtain the phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin. As phenolate and degradation of lignin are carried out in advance, the phenolic hydroxyl group content of lignin is improved. Moreover, high-activity resorcinol is added, so that the prepared lignin-based phenolic resin is high in activity; a foam material made of the modified resin through solidification is high in mechanical properties, and low in scaling off rate. The compression strength of lignin modified phenolic foam is 172.1 kPa, and the bending strength of lignin modified phenolic foam is 254.6 kPa, which are respectively 10.5 percent and 22.1 percent higher than those of foam which is not added with lignin; the scaling off rate of the lignin modified phenolic foam is 19.1 percent, which is 22.8 percent lower than that of the form which is not added with lignin.

Description

technical field [0001] The invention relates to a preparation method of a lignin-modified phenolic resin, specifically phenolizing and degrading lignin under alkaline conditions, and then using the phenolized and degraded lignin to modify a resorcinol-phenol-formaldehyde resin to prepare a light-weight, environmentally friendly heat preservation foam material. Background technique [0002] my country's forest residue resources have large output and high economic value, but their utilization rate is low at present. How to make full use of biomass resources to prepare biomass-based composite materials is the focus of current research. Lignin resources are one of the important sources of biomass resources. Lignin is an aromatic polymer containing structural units of oxyphenylpropanol or its derivatives. There are a large number of hydroxyl groups in the structural units, which can replace part of phenol as the preparation of phenolic formaldehyde Synthetic raw materials for re...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08G8/24C08G8/22C08G8/10C08G8/04C08H7/00
Inventor 陈日清刘娟夏成龙王春鹏储富祥
Owner 重庆集凯科技服务有限公司
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