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Method for preparing phenolic aldehyde adhesive based on lignin phenolized liquid and application thereof

A technology of lignin phenol and lignin, applied in the direction of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of less reactive sites, inconvenient sizing process, complex molecular structure, etc. Achieve good fluidity and storage stability, simple and convenient construction performance, and low free formaldehyde content

Inactive Publication Date: 2008-09-10
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason is that the molecular structure of natural lignin is complex, the molecular weight is high, and the substituents on the aromatic ring of lignin itself are relatively hindered, which cannot effectively react with phenolic resin, and hinder the normal polymerization of phenol and formaldehyde.
The quality of the phenolic adhesive synthesized by chemical modification such as demethylation and methylolation of lignin has been improved to a certain extent compared with the unmodified one, but the modified lignin adhesive still has problems: high molecular weight, High viscosity brings inconvenience to the sizing process and affects the uniformity of coating and the fluidity of the glue; there are few reactive sites on the lignin phenol ring, and the steric hindrance is obvious, so it is difficult to form deep and firm cross-linking, resulting in gluing Decrease in strength, poor moisture resistance; short pot life, etc., affect the application and promotion of lignin modified adhesives
However, there are still problems in the industrial application of wood or bamboo liquefaction products. Due to the complexity of the composition of natural bamboo and wood, there are still some products that cannot be liquefied in the liquefaction products, and the liquefaction efficiency cannot reach 100%. In the patents listed above and Many papers published by the inventor mentioned that the liquefied product must be further filtered and separated before it can be used for the preparation of adhesives, which limits the utilization of the liquefied product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 10.0g of high boiling alcohol lignin to 30.0g of phenol, heat to 130°C and keep it warm for 60 minutes, cool to below 60°C, add 18.0g of 33% lye (6.0g of potassium hydroxide dissolved in 12.0mL of water), Then add 45.0g of 37% formaldehyde, heat up to 95°C after 15 minutes of self-reaction, keep the temperature for 30 minutes, then cool down to 70°C, add 10.0g of 37% formaldehyde, heat up to 94°C after 10 minutes of self-reaction and keep warm, every 3~ After 5 minutes, measure its viscosity with the bubble-reversal method (the viscosity should be controlled at about 3-6S), stop the reaction when it reaches the requirement, and add 20.0mL of water, wait until it is cooled to below 50°C, and discharge.

Embodiment 2

[0028] Heat 53.3g of phenol to 45°C, add 26.7g of sodium lignosulfonate and 3.0mL of concentrated sulfuric acid, rapidly raise the temperature to 120°C (10°C / min), keep the temperature for 20min, cool down to below 60°C, and add 30% lye 41.0g (12.5g of sodium hydroxide dissolved in 28.5mL of water), then add 63.0g of 36% formaldehyde, heat up to 78°C after 20 minutes of self-reaction, then add 45.0g of 36% formaldehyde, and heat up to 78°C after 10 minutes of self-reaction 94°C, heat preservation reaction for 25 minutes, then lower the temperature to 75°C, add 20.0g of 36% formaldehyde, heat up to 92°C, heat preservation reaction, at intervals of 3 to 5 minutes, measure the viscosity with the reverse bubble method (the viscosity is controlled at about 3-8S) , when the requirements are met, stop the heating reaction, add 65.0mL of water, wait until it is cooled to below 50°C, and discharge.

Embodiment 3

[0030] Heat 69.0g of phenol to 100°C, add 23.0g of high boiling alcohol lignin and 5.0mL of concentrated hydrochloric acid, raise the temperature to 115°C, keep the temperature for 10min, cool down to below 55°C, add 46.7g of 30% lye (14.0g of hydroxide Dissolve sodium in 32.7mL of water), then add 63.4g of 37% formaldehyde, heat up to 80°C after 20 minutes of self-reaction, then add 49.3g of 37% formaldehyde, heat up to 94°C after 15 minutes of self-reaction, keep the temperature for 30min, Then lower the temperature to 75°C, add 28.2g of 37% formaldehyde, raise the temperature to 92°C and keep it warm for reaction, every 3 to 5 minutes, measure its viscosity with the reverse bubble method (the viscosity should be controlled at about 3-8S), and stop the heating reaction when the requirement is met , add 200.0mL of water, wait until it is cooled to below 50°C, and discharge.

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Abstract

The invention provides a preparation method for phenolic adhesive based on lignin phenolization liquid and application thereof. Under the condition of normal pressure heating or thermalcatalysis, phenol is taken as liquefaction reagent, lignin is added, the temperature is raised to 90 to 150 DEG C, the thermal insulation liquefaction reaction is made to cool to obtain a lignin liquefaction product; basic catalyst and formaldehyde are directly added into the liquefaction liquid, the temperature is raised to 70 to 97 DEG C under normal pressure to react for 1 to 3 hours, the reaction is terminated when the viscosity is measured to meet the preset requirement, and low-free formaldehyde environmental protection type phenolic adhesive based on lignin phenolization liquid is obtained. The adhesive obtained by the invention has lower cost and lower content of free formaldehyde than the prior phenolic resin adhesive. The plywood pressed by using the adhesive obtained by the invention has good bonding performance.

Description

technical field [0001] The invention belongs to the technical field of adhesives, and in particular relates to a preparation method and an application thereof for synthesizing phenolic adhesives by using lignin phenolization liquid. Background technique [0002] Lignin is one of the three major components of plant fiber raw materials (cellulose, hemicellulose and lignin). A non-petroleum source of renewable aromatic-based compounds. Industrial lignin is mainly derived from the waste liquid of the paper and pulp industry, so it has the advantages of cheap, renewable and environmentally friendly. It is generally believed that the chemical structure of lignin is a complex compound composed of phenylpropane structural units, and the structural units are linked together by ether bonds and C-C bonds to form a random polymer of natural phenols with a three-dimensional structure. There are phenolic hydroxyl groups and aldehyde groups in lignin molecules, and they have certain reac...

Claims

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Application Information

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IPC IPC(8): C09J161/14
Inventor 方红霞张雷吴强林
Owner HUANGSHAN UNIV
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