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Preparation method of phosphorus-containing bisphenol A phenol formaldehyde resin

A technology of phenolic resin and phosphorus bisphenol, which is applied in the field of preparation of organic polymer compounds, can solve problems affecting health and the environment, severe toxicity, etc., and achieve the effects of good product performance, simple preparation process, and excellent flame retardancy

Active Publication Date: 2014-04-16
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, to manufacture flame-retardant epoxy resin composite materials, halogen-containing compounds, especially bromine-containing epoxy resins or curing agents, have been used for a long time, and they are used in conjunction with antimony trioxide flame retardants that are carcinogenic. Bromine compounds will produce corrosive free radicals and hydrogen bromide during combustion, and aromatic compounds with high bromine content will produce highly toxic brominated furans and brominated dioxins, seriously affecting health and the environment

Method used

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  • Preparation method of phosphorus-containing bisphenol A phenol formaldehyde resin
  • Preparation method of phosphorus-containing bisphenol A phenol formaldehyde resin
  • Preparation method of phosphorus-containing bisphenol A phenol formaldehyde resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0037] In a reactor A equipped with a reflux condenser, stirring, and thermocouple, add 216kg DOPO and 600kg xylene, heat up to 90°C, then add 32.6kg paraformaldehyde under stirring, and then react under stirring for 6 hours. The product DOPOM was precipitated and filtered after cooling and precipitation. Then add an appropriate amount of mixed solvent of xylene and ethanol (volume ratio 1:1) to recrystallize 3 times. Obtain DOPOM finished product 226.3kg after drying, productive rate 92%.

Embodiment 1-2

[0039]In a reactor A equipped with a reflux condenser, stirring, and thermocouple, add 216kg DOPO and 600kg xylene, heat up to 110°C, then add 34.3kg paraformaldehyde under stirring, and then react for 4 hours under stirring, The product DOPOM was precipitated and filtered after cooling and precipitation. Then recrystallize three times with a mixed solvent of xylene and ethanol (volume ratio 1:1). Obtain DOPOM finished product 236kg after drying, productive rate 96%.

Embodiment 1-3

[0041] In a reactor A equipped with a reflux condenser, stirring, and thermocouple, add 216kg DOPO and 600kg xylene, raise the temperature to 120°C, then add 39kg paraformaldehyde under stirring, and react for 2 hours under stirring, the product DOPOM was precipitated, filtered after cooling and precipitated. Recrystallize three times with a mixed solvent of xylene and ethanol (volume ratio 1:1). After drying, 239 kg of DOPOM product is obtained, with a yield of 97.2%.

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Abstract

The invention discloses a preparation method of a phosphorus-containing bisphenol A phenol formaldehyde resin, which is characterized by comprising the following components: stirring 216 parts by mass of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 600 parts by mass of dimethylbenzene and 30-60 parts by mass of aldehyde compounds at 90-120 DEG C to react to obtain 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide derivatives; and stirring 228 parts of linear bisphenol A phenol formaldehyde resin, 103-738 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide derivatives and 0.23-23 parts of catalyst at 100-220 DEG C to react, cooling, adding n-butanol, mixing, extracting with water, and distilling to remove the n-butanol, thereby obtaining the phosphorus-containing bisphenol A phenol formaldehyde resin. The phosphorus-containing bisphenol A phenol formaldehyde resin prepared by the method is suitable to be used as a reactive flame retardant for epoxy resins and benzoxazine resins, and can also be used as a curing agent for epoxy resins.

Description

technical field [0001] The invention belongs to the preparation of organic polymer compounds, and relates to a preparation method of phosphorus-containing bisphenol A phenolic resin. The phosphorus-containing bisphenol A phenolic resin prepared by the invention has good flame retardancy, and is suitable for use as a reactive flame retardant for epoxy resins and benzoxazine resins, and also as a curing agent for epoxy resins. Background technique [0002] Composite materials, because of their easy processability, high safety, excellent mechanical properties and heat resistance, are widely used in casting, impregnation, lamination, adhesives, coatings and other purposes. Especially epoxy resin composite materials, because epoxy resin has strong adhesion to glass fiber cloth and other reinforcing materials, and has no volatile matter and small molding shrinkage during curing, so it has a wide range of applications, high mechanical strength, and good electrical insulation. , Go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G59/14C08G59/62
Inventor 代三威徐康林陈小强
Owner SICHUAN DONGFANG INSULATING MATERIAL
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