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

A technology of phenolic resin and formaldehyde, which is applied in the field of preparation methods and prepared products, can solve the problems of affecting crosslinking density, affecting heat resistance, and impossibility to improve impact strength, etc., and achieves the effect of simple preparation method and low pollution

Active Publication Date: 2015-07-01
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] Add 10 parts by weight of phenol, 2 parts of nonylphenol, 8 parts of formaldehyde (38wt% solution), and 0.2 part of oxalic acid into a four-necked flask equipped with a stirrer, a condenser tube, a thermometer and a nitrogen port, and stir (stir The speed is 300rpm) and nitrogen gas is passed through, and the temperature is raised to 100°C for reflux reaction 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 water. The condensation reflux device is connected to a water separator, and the liquid produced by condensation is layered in the water separator. The lower layer is water, and the upper organic layer was returned to the reaction system. The etherification reaction stopped until no water was separated out, and the etherification reaction time was 10 hours, and then added 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO ) 8 ...

Embodiment 2

[0028] Add 10 parts by weight of bisphenol A, 2 parts of nonylphenol, 8 parts of formaldehyde (38wt%), and 0.2 parts of oxalic acid into a four-necked flask equipped with a stirrer, a condenser, a thermometer and a nitrogen port and stir (the stirring speed is 300rpm) and nitrogen gas was introduced, and the temperature was raised to 100°C for reflux reaction for 6 hours. Add 13. parts of n-butanol to carry out etherification reaction. The etherification temperature is controlled at 110°C, and the water is removed by solvent reflux until no more water is produced. The etherification reaction time is 8 hours, and then 9,10-dihydro-9-oxa-10-phospha Heat 8 parts of phenanthrene-10-oxide (DOPO) to 160°C and continue to react for 4 hours, add 8 parts of solvent methyl isobutyl ketone to adjust the viscosity, and obtain a high-performance phenolic formaldehyde with a viscosity of 650cp / 25°C and a phosphorus content of 9.5%. resin.

Embodiment 3

[0030] Add 10 parts by weight of phenol, 1 part of nonylphenol, 8 parts of formaldehyde (38wt%), and 0.2 parts of oxalic acid into a four-necked flask equipped with a stirrer, a condenser tube, a thermometer and a nitrogen port, and stir (the stirring speed is 300rpm) and nitrogen gas, heated to 100°C and refluxed for 6 hours, added 15 parts of n-butanol to control the etherification temperature at 110°C, and used the solvent reflux method to remove moisture until no more moisture was produced. The etherification reaction time was 12 hours, then add 8 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), raise the temperature to 160°C, continue the reaction for 4 hours, add the solvent ethylene glycol Adjust the viscosity with 8 parts of ether 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 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 rings. Common phenolic resins are very brittle and have poor toughness. As a result, phenolic resin products have low impact strength and short service life. In the application of copper clad laminates, the cost is increased and the cost is greatly increased. The application of phenolic resin is limited. [0003] Epoxy resin has high tensile strength and modulus, low curing shrinkage, good moisture resistance, chemica...

Claims

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Application Information

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Patent Type & Authority Patents(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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