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Purification method of modified burning-resistant phenolic resin

A technology of phenolic resin and purification method, which is applied in the field of phenolic resin purification, can solve the problems of affecting product quality, poor burning resistance, and endangering the health of on-site operators, so as to reduce the content of free aldehydes and free phenols and improve burning resistance. Good burning effect, suitable for large-scale industrial production

Inactive Publication Date: 2022-01-07
王顺方
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Phenolic resin is made by polycondensation reaction of phenols and aldehydes under the action of a catalyst. In the current phenolic resin synthesis process, the product still contains a relatively high content of free phenol and free aldehyde monomers. If conventional distillation methods are used It is difficult to remove free phenol and free aldehyde monomers from phenolic resin. These impurities seriously affect the quality of the product, especially the poor burning resistance, and also endanger the health of on-site workers.

Method used

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  • Purification method of modified burning-resistant phenolic resin
  • Purification method of modified burning-resistant phenolic resin

Examples

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Effect test

Embodiment 1

[0024] A kind of purification method of modified burning-resistant phenolic resin, comprises the steps:

[0025] S1. Dissolve 1 kg of lignin in 10 kg of dioxane, add 1 kg of sodium hydroxide and 1 kg of n-hexadecanol under nitrogen protection, stir for 1 hour, the stirring speed is 100 r / min, the stirring temperature is 90 ° C, and adjust the pH value of the system 3, centrifuged, washed with n-hexane, filtered, and dried to obtain modified lignin;

[0026] S2. Stir 20kg of xylenol, 1kg of modified lignin, and 1kg of sodium hydroxide at room temperature for 5 minutes at a stirring speed of 100r / min, slowly raise the temperature to 80°C at a heating rate of 0.5°C / min, and add dropwise under stirring 30kg mass fraction is 30% formaldehyde solution, continue to stir for 1h, obtain prefabricated material;

[0027] S3. Add the prefabricated material into the reaction kettle, vacuum dehydrate under normal pressure, the vacuum degree is 10kPa, and keep the temperature at 120°C to ob...

Embodiment 2

[0030] A kind of purification method of modified burning-resistant phenolic resin, comprises the steps:

[0031] S1. Dissolve 5kg of lignin in 30kg of dioxane, add 2kg of sodium tert-butoxide and 3kg of n-hexadecanol under nitrogen protection, stir for 3 hours, the stirring speed is 300r / min, the stirring temperature is 110°C, and adjust the pH of the system value is 5, centrifuged, washed with n-hexane, filtered, and dried to obtain modified lignin;

[0032] S2. Stir 40kg of phenol ether, 4kg of modified lignin, and 2kg of potassium hydroxide at room temperature for 20min at a stirring speed of 300r / min, slowly raise the temperature to 90°C at a heating rate of 2°C / min, and add 60kg dropwise under stirring The mass fraction is 35% formaldehyde solution, and the stirring is continued for 2 hours to obtain the prefabricated material;

[0033] S3. Add the prefabricated material into the reaction kettle, vacuum dehydrate under normal pressure, the vacuum degree is 50kPa, and kee...

Embodiment 3

[0036] A kind of purification method of modified burning-resistant phenolic resin, comprises the steps:

[0037] S1. Dissolve 2kg of lignin in 15kg of dioxane, add 1.2kg of sodium methoxide and 1.5kg of cetyl alcohol under nitrogen protection, stir for 1.5h, the stirring speed is 150r / min, the stirring temperature is 95°C, adjust the system The pH value is 3.5, centrifuged, washed with n-hexane, filtered, and dried to obtain modified lignin;

[0038] S2. Stir 25kg of naphthol, 1.5kg of modified lignin, and 1.2kg of ammonia water at room temperature for 10 minutes at a stirring speed of 120r / min, slowly raise the temperature to 82°C at a heating rate of 1°C / min, and add 35kg dropwise under stirring The mass fraction is 31% formaldehyde solution, and the stirring is continued for 1.2h to obtain the prefabricated material;

[0039] S3. Add the prefabricated material into the reaction kettle, vacuum dehydrate under normal pressure, the vacuum degree is 20kPa, and keep the tempera...

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Abstract

The invention discloses a purification method of modified burning-resistant phenolic resin, which comprises the following steps: dissolving lignin in dioxane, adding a first catalyst and n-hexadecanol under the protection of nitrogen, conducting stirring, adjusting the pH value of the system to 3-5, centrifugally conducting separating, and conducting washing, filtering and drying to obtain modified lignin; mixing a phenolic compound, the modified lignin and a second catalyst, conducting stirring at room temperature, slowly conducting heating to 80-90 DEG C, dropwise adding a formaldehyde solution in a stirring state, and continuously conducting stirring to obtain a prefabricated material; adding the prefabricated material into a reaction kettle, and performing vacuum dehydration in a normal pressure state to obtain a dehydrated prefabricated material; and transferring the dehydrated prefabricated material to a molecular distiller for distillation treatment, keeping the pressure intensity in the molecular distiller at 10-20kPa, and collecting the phenolic resin product by using a collection bottle. The environment pollution is effectively reduced, the burning resistance of the phenolic resin can be effectively enhanced, the product quality can be greatly improved, and the method is particularly suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of purification of phenolic resins, in particular to a purification method of modified burn-resistant phenolic resins. Background technique [0002] Phenolic resin is a general term for resins formed by the reaction of phenols and aldehydes in the presence of catalysts. Among them, thermosetting phenolic resins formed by phenol and formaldehyde under alkaline catalyst conditions are the most common, and thermosetting phenolic resin products have good dimensional stability. , acid resistance, mechanical properties and heat resistance, widely used in transportation, construction, military, mining and other industries. [0003] Phenolic resin is made by polycondensation reaction of phenols and aldehydes under the action of a catalyst. In the current phenolic resin synthesis process, the product still contains a relatively high content of free phenol and free aldehyde monomers. If conventional distillation metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/34
CPCC08G8/34
Inventor 王顺方
Owner 王顺方
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