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Preparation method of phosphorous-containing phenol formaldehyde resin and resin prepared

A technology of phenolic resin and formaldehyde, applied in the field of preparation methods and prepared products, can solve the problems of affecting heat resistance, affecting cross-linking density, impact strength cannot be improved, etc., and achieves the effect of less pollution and simple preparation method

Active Publication Date: 2013-06-26
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Epoxy resin composition is usually composed of epoxy resin and curing agent. If phosphorus is introduced through the reaction of epoxy resin and phosphorus-containing compounds, the density of epoxy functional groups will be reduced, which will affect the cross-linking density, thereby affecting its heat resistance. Performance, impact strength can not be improved

Method used

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  • Preparation method of phosphorous-containing phenol formaldehyde resin and resin prepared

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 10 parts by weight of phenol, 2 parts of nonylphenol, 8 parts of formaldehyde (38wt% solution), and 0.2 part of oxalic acid were added to the four-necked flask equipped with a stirrer, a condenser, a thermometer and a nitrogen interface, and stirred (stirred). The speed is 300 rpm) and nitrogen is passed through, and the temperature is raised to 100 °C and refluxed for 6 hours.

[0026] Add 14 parts of n-butanol to carry out etherification reaction, the etherification temperature is controlled at 110 ° C, the solvent reflux method is used to remove moisture, the device for condensation reflux is connected to a water separator, and the liquid produced by condensation is layered in the water separator, and the lower layer is water, and the upper organic layer was returned to the reaction system. The etherification reaction was stopped until there was no more water to separate out. The etherification reaction time was 10 hours, and then 9,10-dihydro-9-oxa-10-phosphaphenant...

Embodiment 2

[0028] 10 parts by weight of bisphenol A, 2 parts of nonylphenol, 8 parts of formaldehyde (38wt%), and 0.2 part of oxalic acid were added to the four-necked flask equipped with a stirrer, a condenser, a thermometer and a nitrogen interface and stirred (stirring speed was 300 rpm) and nitrogen was introduced, the temperature was raised to 100 °C and the reaction was refluxed for 6 hours. 13. parts of n-butanols were added, and etherification reaction was performed. The etherification temperature was controlled at 110°C, and the water was removed by the solvent reflux method until no more water was produced. The etherification reaction time was 8 hours, and then 9,10-dihydro-9-oxa-10-phosphine was added. 8 parts of phenanthrene-10-oxide (DOPO) was heated to 160°C and continued to react for 4 hours, and 8 parts of methyl isobutyl ketone was added to adjust the viscosity to obtain a high-performance phenolic with a viscosity of 650cp / 25°C and a phosphorus content of 9.5%. resin. ...

Embodiment 3

[0030] 10 parts of phenol, 1 part of nonylphenol, 8 parts of formaldehyde (38wt%), and 0.2 part of oxalic acid in parts by weight were added to the four-necked flask equipped with a stirrer, a condenser, a thermometer and a nitrogen interface, and stirred (stirring speed was 300rpm) and nitrogen was introduced, the temperature was raised to 100°C for reflux reaction for 6 hours, 15 parts of n-butanol was added and the etherification temperature was controlled at 110°C, and the water was removed by the solvent reflux method until no more water was produced. The etherification reaction time was 12 hours, then add 8 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), heat up to 160°C, continue to react for 4 hours, add solvent ethylene glycol methyl 8 parts of ether to adjust the viscosity to obtain a high-performance phenolic resin with a phosphorus content of 9.5%.

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Abstract

The invention provides a preparation method of phosphorous-containing phenol formaldehyde resin. The preparation method comprises the following steps: mixing mixture of two phenols with acidic catalysts and formaldehyde, and increasing the temperature of a reaction system to 50-120 DEG C and reacting for 3-8 hours; 2) adding alcohol for performing etherification reaction, and controlling the etherification temperature to be 100-150 DEG C; 3) adding organic phosphorus compounds, increasing the temperature of the reaction system, and reacting for 2-5 hours. The phosphorous is introduced in a phenol formaldehyde resin and modified to prepare the high-performance phenol formaldehyde resin, the phenol formaldehyde resin is matched with epoxy resin to be used for copper clad plates, and the flame retardation can achieve UL94V-0. The preparation method is simple, and the synthesis pollution is less. The copper clad plate manufactured by the phenol formaldehyde resin can not produce toxic gas in combustion, thereby being incapable of injuring a human body.

Description

technical field [0001] The invention belongs to the field of organic polymer compounds, and in particular relates to a preparation method of a phosphorus-containing phenolic resin and a prepared product. Background technique [0002] Phenolic resin has the advantages of simple production process, low price, good heat resistance, electrical insulation, corrosion resistance, flame retardancy, dimensional stability, etc., and is a research and development hotspot in this field. However, the molecular structure of phenolic resin contains a rigid structure of benzene ring. The common phenolic resin is very brittle and has poor toughness, so that the impact strength of phenolic resin products is low and the service life is short, which increases the cost in the application of copper clad laminates. limited the application of phenolic resins. [0003] Epoxy resin has high tensile strength and modulus, low curing shrinkage, good moisture resistance, chemical resistance and electric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/36C08G8/28C08G59/62B32B15/092B32B27/04
Inventor 江成真李枝芳刘耀张淑娇
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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