Preparation method of novel phosphorus-containing biphenyl novolac epoxy resin and condensate of novel phosphorus-containing biphenyl novolac epoxy resin

A technology of biphenyl novolac epoxy resin and phenol novolac epoxy resin, which is applied in the chemical industry, can solve the problems of corrosion of electronic components, dissociation of halides, human body harm, etc., and achieves low water absorption, excellent heat resistance and flame retardancy. The effect is simple and easy to operate

Inactive Publication Date: 2011-08-31
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the most widely used bromine-containing epoxy resin has excellent flame retardant effect, but long-term use at high temperature will cause halide dissociation, which may cause corrosion to electronic components
And when the halogen-containing compound burns, it will produce carcinogenic substances harmful to the environment and human body

Method used

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  • Preparation method of novel phosphorus-containing biphenyl novolac epoxy resin and condensate of novel phosphorus-containing biphenyl novolac epoxy resin
  • Preparation method of novel phosphorus-containing biphenyl novolac epoxy resin and condensate of novel phosphorus-containing biphenyl novolac epoxy resin
  • Preparation method of novel phosphorus-containing biphenyl novolac epoxy resin and condensate of novel phosphorus-containing biphenyl novolac epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] like figure 1 As shown, the process route of this embodiment is as shown in the figure.

[0064] Step 1, add 24.2 parts of 4,4'-biphenyl dimethyl dimethyl ether and 87 parts of methyl butyl ketone in a four-necked flask with a thermometer, a stirring device and a condenser. Add 34 parts of p-phenylbiphenol into a four-necked flask in batches, stir and raise the temperature to 135°C, and maintain the reaction for 4 hours to remove methyl butyl ketone to obtain a biphenol-formaldehyde resin.

[0065] Step 2: add 15 parts of biphenyl novolac resins, 42.4 parts of epoxy chlorohydrin and 2.28 parts of NaOH solution (biphenyl novolac resins: epoxy chlorohydrin: hydroxide Sodium molar ratio 1:10:1), reacted at 65°C for 4h. Afterwards, the organic layer was taken by liquid separation, and the solvent was removed under reduced pressure to obtain the product.

[0066] Step 3, add 6 parts of biphenyl novolac epoxy resins, 1.94 parts of 10-(2,5-dihydroxyphenyl)-10-dihydro-9- Ox...

Embodiment 2

[0072] Step 1, add 24.2 parts of 4,4'-biphenyl dimethyl dimethyl ether and 87 parts of dichloroethane in a four-necked flask with a thermometer, a stirring device and a condenser. Add 34 parts of p-phenylbiphenol into the reaction bottle in batches, stir and raise the temperature to 80°C, and maintain the reaction for 8 hours, and discharge while hot to obtain biphenol novolac resin.

[0073] Step 2: add 15 parts of biphenyl phenolic resins, 53.01 parts of epoxy chlorohydrin and 2.28 parts of sodium hydroxide (biphenyl phenolic resins: epoxy chlorohydrin: hydrogen Sodium oxide molar ratio 1:10:1), react at 65°C for 4h, separate the liquid to take the organic layer, and remove the solvent under reduced pressure to obtain the product.

[0074] Step 3, add 6 parts of biphenyl novolac epoxy resin, 1.46 parts of 10-(2,5-dihydroxyphenyl)-10-dihydro-9- Oxa-10-phosphaphenanthrene-10-oxide (biphenol novolac epoxy resin and 10-(2,5-dihydroxyphenyl)-10-dihydro-9-oxa-10-phosphaphenanthre...

Embodiment 3

[0076] Step 1, add 24.2 parts of 4,4'-biphenyl dimethyl dimethyl ether and 87 parts of methyl isobutyl ketone in a four-necked flask with a thermometer, a stirring device and a condenser tube, and 34 parts of p-phenyl biphenyl Phenol was added to the reaction flask in batches, and the temperature was raised to 115°C with stirring, and the reaction was maintained for 5 hours, and the solvent was removed to obtain a biphenol-formaldehyde resin.

[0077] Step 2: add 15 parts of biphenyl phenolic resins, 63.62 parts of epoxy chlorohydrin and 2.28 parts of sodium hydroxide (biphenyl phenolic resins: epoxy chlorohydrin: hydrogen Sodium oxide molar ratio (1:12:1), react at 75°C for 4h, separate liquid to take the organic layer, and remove the solvent under reduced pressure to obtain the product.

[0078] Step 3, add 6 parts of biphenol novolac epoxy resin, 2.18 parts of 10-(2,5-dihydroxyphenyl)-10-dihydro-9- Oxa-10-phosphaphenanthrene-10-oxide (biphenol novolac epoxy resin and 10-(2...

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Abstract

The invention relates to a preparation method of novel phosphorus-containing biphenyl novolac epoxy resin and condensate of the novel phosphorus-containing biphenyl novolac epoxy resin. The preparation method of the resin comprises the following steps of: dissolving 4,4'-bipheyl dimethyl dimethyl ether and p-phenylphenol in an organic solvent; heating to reach the temperature of between 60 DEC and 180 DEG C to react for 3 to 8 hours so as to prepare biphenyl novolac resin; performing epoxidation under the action of a base catalyst and keeping a reaction temperature at 50 DEG C to 80 DEG C for 2 to 3 hours to prepare biphenyl novolac epoxy resin; and reacting the biphenyl novolac epoxy resin with a phosphorus-containing activated monomer to prepare the novel phosphorus-containing biphenyl novolac epoxy resin. The phosphorus-containing biphenyl novolac epoxy resin has superior flame retardant property, heat resistance and water resistance; and the preparation method is simple and feasible. The epoxy resin is suitable to be used as a sealing material and an adhesive used in electronic elements and an electric insulating material used in an electronic circuit substrate.

Description

technical field [0001] The invention relates to a method for preparing novel phosphorous-containing biphenyl novolac epoxy resin and its cured product in the technical field of chemical industry. The epoxy resin is suitable as a sealing material and adhesive used in electronic components, and an electrical insulating material used in electronic circuit substrates. Background technique [0002] Epoxy resin has comprehensive properties such as excellent adhesion, electrical insulation, dielectric, chemical stability and small shrinkage, and is widely used in the fields of electronics, light industry, construction, machinery, aerospace and other fields. Among them, the epoxy resin plastic packaging materials used in electronic components and electronic instruments are strongly required to prevent and delay fire. So far, the most widely used bromine-containing epoxy resin has excellent flame retardant effect, but long-term use at high temperature will cause halide dissociation,...

Claims

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Application Information

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IPC IPC(8): C08G59/14C08G59/06C08L63/04C08G59/62C09K3/10C09J163/04H05K1/03
Inventor 夏新年刘甲熊远钦徐伟箭曾小亮
Owner HUNAN UNIV
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