Method for preparing thermoset phenolic resin and method for preparing conductive slurry

A technology of phenolic resin and phenolic resin solution, which is applied in the field of preparation of low-temperature conductive paste, thermosetting phenolic resin, and phenolic resin. rate, the effect of increasing consumption

Active Publication Date: 2012-07-18
广州三则电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cured low-temperature conductive paste is prone to pores, severe moisture absorption, unstable

Method used

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  • Method for preparing thermoset phenolic resin and method for preparing conductive slurry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Add 40 grams of phenol, 41.4 grams of 37% formaldehyde, 0.85 grams of sodium hydroxide and 1.81 grams of barium hydroxide in the reaction bottle, and react at a constant temperature of 60°C for 5 hours, then add 27.6 grams of 37% formaldehyde and react at a constant temperature of 60°C After 5 hours, 4.17 g of 50% sulfuric acid was added for 10 minutes of neutralization reaction, and then 60 g of cyclohexanone and 20 g of toluene were added for extraction and washed twice with water, and the water phase was removed. The solution was transferred to a new reaction vial and vacuum desolvated at 115°C for 1.5 hours. Finally, ethylene glycol monobutyl ether is added for dissolution to obtain a thermosetting phenolic resin solution with a solid content of about 70%. Described phenolic resin is carried out the mensuration of free phenol, free formaldehyde and water content, and its result is shown in Table 1. Use the thermosetting phenolic resin solution as a bonding material,...

Embodiment 2

[0037] Add 40 grams of phenol, 41.4 grams of 37% formaldehyde, 0.85 grams of sodium hydroxide and 0.62 grams of magnesium hydroxide in the reaction flask, and react at a constant temperature of 70 °C for 4 hours, then add 20.7 grams of 37% formaldehyde and react at a constant temperature of 70 °C 4h, 7.76 g of 20% hydrochloric acid was added for 10 minutes of neutralization reaction, and then 80 g of cyclohexanone was added for extraction and washed twice with water, and the water phase was removed. The solution was transferred to a new reaction vial and vacuum desolvated at 110°C for 1.5 hours. Finally, ethylene glycol butyl ether acetate was added for dissolution to obtain a thermosetting phenolic resin solution with a solid content of 70%. Described phenolic resin is carried out the mensuration of free phenol, free formaldehyde and water content, and its result is shown in Table 1. Use the thermosetting phenolic resin solution as the bonding material, adopt conductive carb...

Embodiment 3

[0039] Add 40 grams of phenol, 34.51 grams of 37% formaldehyde, 0.6 grams of potassium hydroxide and 1.23 grams of barium hydroxide in the reaction bottle, and react at a constant temperature of 90 ° C for 3 hours, then add 20.7 grams of 37 % formaldehyde and react at a constant temperature of 90 ° C 3h, 3.13g of 50% sulfuric acid was added for 10 minutes of neutralization reaction, then 80g of cyclohexanone was added for extraction and washed twice with water, and the water phase was removed. The solution was transferred to a new reaction vial and vacuum desolvated at 108°C for 1.5 hours. Finally, diethylene glycol monomethyl ether is added for dissolution to obtain a thermosetting phenolic resin solution with a solid content of about 70%. Described phenolic resin is carried out the mensuration of free phenol, free formaldehyde and water content, and its result is shown in Table 1. Use the thermosetting phenolic resin solution as the bonding material, adopt the silver-coated...

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Abstract

The invention provides a method for preparing thermoset phenolic resin and a method for preparing conductive slurry. The method for preparing the thermoset phenolic resin comprises the following steps of: firstly weighing phenol, a part of methanal, and a mixed alkaline catalyst and reacting for several hours in a reaction flask at 50-90 DEG C; adding the residual methanal to the reaction flask to react; adding acid for neutralizing, and carrying out extraction separation; heating and vacuumizing for removing agents, adding an organic solvent for dissolving to obtain a thermoset phenolic resin solution. According to the method for preparing the thermoset phenolic resin, with the mixed alkaline as a catalyst, backflow reaction is performed for a period of time and then the acid is added for neutralizing; then the organic solvent with very low water solubility is added to carry out extraction separation; then, the solvents are removed in vacuum by heating; and finally the organic solvent is added for dissolving to obtain the thermoset phenolic resin solution with a certain solid content. In addition, a conductive filler, organic diluent and other additives are added to the prepared thermoset phenolic resin solution at the same time to obtain the low-temperature conductive slurry which has the advantages of high conductivity, extremely high adhesion strength and stable electric performance and is suitable for screen printing.

Description

technical field [0001] The invention relates to a preparation method of a phenolic resin, more precisely, relates to a preparation method of a thermosetting phenolic resin and a method for preparing a low-temperature conductive paste therefrom, belonging to the field of conductive electronic materials. Background technique [0002] Thermosetting phenolic resins are usually formed by the reaction of phenols and aldehydes in the presence of alkaline catalysts, among which thermosetting phenolic resins formed from phenol and formaldehyde under alkaline conditions are the most common. Thermosetting phenolic resin has good dimensional stability, flame retardancy, corrosion resistance, high temperature resistance, insulation and machining properties, and can be used in the manufacture of copper clad laminates, plastic materials, laminated plastics, foam materials for printed circuit boards , honeycomb plastics, etc., can also be used as paint raw materials, adhesives, anti-corrosi...

Claims

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Application Information

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IPC IPC(8): C08G8/10H01B1/22H01B1/24C08L61/10C08K13/02
Inventor 陈建权
Owner 广州三则电子材料有限公司
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