Lignin phenol resin prepolymer and preparation method thereof, lignin phenol resin and preparation method thereof

A technology of phenolic resin prepolymerization and phenolic resin, applied in the field of lignin phenolic resin prepolymer and its preparation, lignin phenolic resin and its preparation, can solve the problems of low chemical reactivity, poor fluidity and heat resistance of phenolic resin, Low strength and other problems, to achieve the effect of improving reactivity, fluidity, good heat resistance and high strength

Active Publication Date: 2013-04-10
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when using this method to prepare lignin-modified phenolic resin, the chemical reactivity of lignin molecules is low, and the obtained modified phenolic resin has poor fluidity and heat resistance, so it is applied to wear-resistant materials such as grinding wheels. When in the material, the strength is lower

Method used

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preparation example Construction

[0021] The invention provides a kind of preparation method of lignin phenolic resin prepolymer, comprises the following steps:

[0022] A) Mix lignin compounds, phenolic compounds and acidic catalysts, heat to 180~350°C for reaction, and obtain mixed reaction liquid;

[0023] B) mixing the mixed reaction liquid with formaldehyde, and obtaining a lignin phenolic resin prepolymer after polycondensation reaction.

[0024] In the present invention, the lignin compound, the phenolic compound and the acidic catalyst are firstly mixed, heated to 180-350° C. for reaction, and a mixed reaction solution is obtained. In the present invention, the mixed reaction solution is obtained according to the following specific methods:

[0025] mixing the lignin compound, the phenolic compound and the acidic catalyst into a high-pressure reactor, and replacing the air in the high-pressure reactor with high-purity nitrogen;

[0026] The high-pressure reactor is heated to 180-350° C., and the lign...

Embodiment 1

[0042] Put 1000g of phenol and 100g of calcium lignosulfonate into the autoclave, add 10g of catalyst phosphoric acid, and then pass high-purity nitrogen into the autoclave for 5 minutes to replace the air in the autoclave. Close the autoclave after the nitrogen gas is ventilated, stir the mixture and heat up to 180°C for cracking and phenolization reaction for 1 hour, after 1 hour, cool the autoclave to 90°C, add 20g of oxalic acid, and add the concentration dropwise at this temperature It is 671.9g of 38% formaldehyde. After dropping the formaldehyde, carry out polycondensation reaction at 100°C for 1 hour. After the reaction, excess water and phenol are removed to obtain lignin phenolic resin prepolymer.

Embodiment 2

[0044] Put 1000g of phenol and 2000g of alkali lignin into the autoclave, add 20g of catalyst sulfuric acid, and then pass high-purity nitrogen into the autoclave for 5 minutes to replace the air in the autoclave. Close the autoclave after the nitrogen gas is passed, stir the mixture and heat up to 250°C for cracking and phenolization reaction for 2 hours, after 2 hours, cool the autoclave to 90°C, and add formaldehyde with a concentration of 38% dropwise at this temperature 83.99g, polycondensation reaction at 100°C for 1 hour after dropping the formaldehyde, and remove excess water and phenol after the reaction to obtain lignin phenolic resin prepolymer.

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Abstract

The invention provides a preparation method of lignin phenol resin prepolymer, which comprises the following steps: mixing lignin compound, phenolic compound and acid catalyst, and heating the mixture to be 180 to 350 DEG C for reaction so as to obtain mixed reaction liquid; and mixing the mixed reaction liquid with formaldehyde, and obtaining lignin phenol resin prepolymer after condensation polymerization. According to the invention, the phenolic compound is used as a solvent, double bonds and ether bonds on the phenolic compound are destroyed through an acid environment provided by the acid catalyst under a high temperature condition of 180 to 350 DEG C, so that the molecular weight of the phenolic compound is reduced; and while a phenol molecule is connected to the hydroxymethyl active group on a lignin, so that the chemical reactivity of a lignin molecule is improved, and the reactivity of the lignin phenol resin prepolymer is improved. Therefore, the obtained lignin phenol resin has good mobility, good heat resistance and high strength.

Description

technical field [0001] The invention belongs to the technical field of phenolic resins, and in particular relates to a lignin phenolic resin prepolymer and a preparation method thereof, a lignin phenolic resin and a preparation method thereof. Background technique [0002] Phenolic resin is also called bakelite, also known as bakelite powder, has good acid resistance, mechanical properties, heat resistance, and is widely used in anti-corrosion engineering, adhesives, flame-retardant materials, grinding wheel manufacturing and other industries. At present, the preparation method of phenolic resin is mainly made by polycondensation of phenol and formaldehyde under catalyst conditions, neutralized and washed with water, but due to the incomplete reaction of phenol and formaldehyde in the above reaction, unreacted phenol and formaldehyde will remain in the phenolic resin. The release of formaldehyde, free phenol and free aldehyde into the air will affect the atmospheric environm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
Inventor 江成真焦峰董岳徐秋实
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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