A kind of epoxy resin containing phenolic hydroxyl group and preparation method of flame-retardant foaming material thereof

A technology of novolac epoxy resin and epoxy resin, which is applied in the field of preparation of epoxy foam, novolac epoxy resin and its foam materials, can solve the problems of low mechanical strength, easy to drop slag and powder, use restrictions, etc., and achieve improvement Effects of cross-linking density, increased reactivity, and uniform foam density distribution

Inactive Publication Date: 2018-08-07
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively low mechanical strength of phenolic foam, its use is also limited to a certain extent because it is easy to drop slag and powder.

Method used

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  • A kind of epoxy resin containing phenolic hydroxyl group and preparation method of flame-retardant foaming material thereof
  • A kind of epoxy resin containing phenolic hydroxyl group and preparation method of flame-retardant foaming material thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of synthesis that contains the epoxy resin of phenolic hydroxyl group, comprises the following steps:

[0033] Add 100g of phenol and 28.7g of paraformaldehyde into a three-necked flask, raise the temperature to 60°C, add 8.51g of NaOH (prepared as a 50% aqueous solution by mass fraction) to catalyze the addition reaction of phenol and formaldehyde, control the temperature at 60°C, and react 2 hour, then raise the temperature to 80°C, keep the heat for 4 hours, then add 109.57g epichlorohydrin at 60°C, control the temperature at 60°C, react until the epoxy resin is neutral, slowly add hot water (40- 50° C.) to wash the resin, and then distill off water and unreacted epichlorohydrin under reduced pressure to obtain an epoxy resin product containing phenolic hydroxyl groups.

[0034] The technical parameters of the obtained epoxy resin product of phenolic hydroxyl group are: viscosity at 25° C. of 8600 mPa·S, solid content of 89.91%, and epoxy value of 0.31 mol / 100...

Embodiment 2

[0036] Prepare a kind of epoxy resin foam material containing phenolic hydroxyl based on embodiment 1 product, comprise the following steps:

[0037] Add 100g of the epoxy resin containing phenolic hydroxyl groups in Example 1, together with 5g Tween-80 and 6g petroleum ether, into the reactor and stir rapidly for 10min, then add 6g of diethylenetriamine curing agent, stir for 1min and then pour into Put it into a mold that has been preheated to 60°C, put it in an oven at 60°C and keep it warm for 2.5 hours, take it out and cool it to room temperature, and then demould to obtain an epoxy resin foam material containing phenolic hydroxyl groups.

[0038] Gained epoxy resin foam material containing phenolic hydroxyl group has even foam cells, and its technical parameters are: oxygen index 32.1%; foam density 0.15g / cm 3 ; Water absorption 3.27%.

Embodiment 3

[0040] A kind of synthesis that contains the epoxy resin of phenolic hydroxyl group, comprises the following steps:

[0041] Add 100g of phenol and 25.5g of paraformaldehyde into a three-necked flask, raise the temperature to 60°C, add 12.76g of NaOH (prepared as a 50% aqueous solution by mass fraction) to catalyze the addition reaction of phenol and formaldehyde, control the temperature at 60°C, and react for 2.5 hour, then raise the temperature to 80°C, heat preservation reaction for 4 hours, then add 98.62g epichlorohydrin at 60°C, control the temperature at 60°C, react until the epoxy resin is neutral, slowly add hot water (40- 50°C) to wash the resin, and then distill off water and unreacted epichlorohydrin under reduced pressure to obtain an epoxy resin containing phenolic hydroxyl groups.

[0042] The technical parameters of the epoxy resin product of the obtained phenolic hydroxyl group are: viscosity at 25° C. of 9800 mPa·S, solid content of 90.62%, and epoxy value of...

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Abstract

The invention discloses an epoxy resin containing phenolic hydroxyl groups and a preparation method of a fire-retardant foam material based on the epoxy resin.The preparation method includes the specific steps that phenol and formaldehyde are synthesized into phenolic resin under the effect of a basic catalyst, the phenolic resin is then reacted with epoxy chloropropane for 2-5 h at 60-100 DEG C so that part of phenolic hydroxyl groups in the phenolic resin can be subjected to an epoxidation reaction, water and unreacted epoxy chloropropane are removed, and the epoxy resin containing phenolic hydroxyl groups is obtained, wherein the epoxide number of the epoxy resin containing phenolic hydroxyl groups is 0.19-0.32 mol / 100 g; then, the fire-retardant foam material is prepared with the obtained epoxy resin containing phenolic hydroxyl groups as the main body, wherein the fire-retardant foam material is prepared from, by weight, 3-8 parts of a surfactant, 80-100 parts of the epoxy resin containing phenolic hydroxyl groups, 4-10 parts of a foaming agent and 10-40 parts of a curing agent.The preparation method is easy and convenient to implement, the polyfunctional epoxy resin containing phenolic hydroxyl groups, epoxy groups, benzene rings and the like is prepared and has the advantages of phenolic resin and the advantages of epoxy resin, and the prepared epoxy resin foam material is excellent in fire retardance, uniform in foam density and low in water absorption and can be applied to the fields of energy saving and heat insulating, fireproof and fire-retardant materials and the like.

Description

technical field [0001] The present invention relates to the preparation method of novolac epoxy resin and foam material thereof, specifically using phenol to prepare epoxy resin containing phenolic hydroxyl group under the action of alkaline catalyst and using it to prepare epoxy foam with excellent flame retardant performance, which belongs to flame retardant heat preservation etc. The field of high-tech materials. Background technique [0002] Epoxy resin is widely used because of its excellent adhesion, electrical insulation properties and low cure shrinkage. Currently, the bisphenol A epoxy resin widely used in the market is a bifunctional epoxy resin, which cannot be involved in the field of high temperature resistant and flame retardant materials because it does not have flame retardancy. [0003] Phenolic resins are widely used in adhesives, molding materials, foam plastics, and ablation-resistant materials because of their excellent heat resistance, flame resistance...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/08C08L63/00C08J9/14C08J9/10
CPCC08G59/08C08J9/102C08J9/141C08J2203/04C08J2203/14C08J2363/00C08L63/00C08L2201/02C08L2203/14
Inventor 张超灿邓玲王延召黄亮
Owner WUHAN UNIV OF TECH
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