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Epoxy resin and preparation method and application thereof

A technology of epoxy resin and methoxy, which is applied in the field of epoxy resin and its preparation, can solve the problems of restricting the application of crystalline epoxy resin, and achieve the effects of low dielectric loss, low processing viscosity and excellent heat resistance

Inactive Publication Date: 2014-03-12
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the actual application process, it is often necessary to heat to a higher temperature before use, which limits the application of crystalline epoxy resin to a large extent.

Method used

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  • Epoxy resin and preparation method and application thereof
  • Epoxy resin and preparation method and application thereof
  • Epoxy resin and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 4'-(3-hydroxyphenoxy)biphenol

[0041] 1) Preparation of 4-methoxy-4'-hydroxybiphenyl

[0042] In a three-neck flask equipped with mechanical stirring, a condenser and a nitrogen inlet and outlet, 187.5 grams (1 mole) of 4,4'-dihydroxybiphenyl was dissolved in 500 milliliters of 10 wt% sodium hydroxide aqueous solution. At room temperature (25° C.), 90 g (1 mole) of methylating reagent dimethyl carbonate was added dropwise in 3 hours. After the reaction, the white solid was filtered and rinsed with 1000 ml of 10 wt% sodium hydroxide aqueous solution. The obtained solid was dissolved in boiling water, and the insoluble matter was removed by hot filtration. At 70°C, adjust the pH of the solution to ≤6 with 20 wt% hydrochloric acid. The resulting white solid was filtered and recrystallized from ethanol to give white crystals. The yield was 52%.

[0043] The structural detection data of this compound are as follows (the proton nuclear magnetic spectrum, mass ...

Embodiment 2

[0065] Example 2 4'-(3-hydroxyphenoxy)biphenol

[0066] 1) Preparation of 4-methoxy-4'-hydroxybiphenyl

[0067] In a three-necked flask equipped with mechanical stirring, a condenser, and a nitrogen inlet and outlet, 93.75 grams (0.5 moles) of 4,4'-dihydroxybiphenyl was dissolved in 500 milliliters of 10% wt sodium hydroxide aqueous solution. At room temperature (25° C.), 63 g (0.5 mol) of methylating reagent dimethyl sulfate was added dropwise in 3 hours. After the reaction, the white solid was filtered and rinsed with 500 ml of 10 wt% sodium hydroxide aqueous solution. The obtained solid was dissolved in boiling water, and the insoluble matter was removed by hot filtration. At 70°C, use 20%wt hydrochloric acid to adjust the pH of the solution to ≤6. The resulting white solid was filtered and recrystallized from ethanol to give white crystals. The yield is 55%.

[0068] The structural detection data of this compound are as follows (the proton nuclear magnetic spectrum, m...

Embodiment 3

[0087] Example 3 4'-(3-hydroxyphenoxy)biphenol

[0088] 1) Preparation of 4-methoxy-4'-hydroxybiphenyl

[0089] In a three-necked flask equipped with mechanical stirring, a condenser and a nitrogen inlet and outlet, 46.88 grams (0.25 moles) of 4,4'-dihydroxybiphenyl was dissolved in 250 milliliters of 8% wt potassium hydroxide aqueous solution. At room temperature (25° C.), 71 g (0.5 mol) of methylating reagent methyl iodide was added dropwise within 3 hours. After the reaction, the white solid was filtered and rinsed with 500 ml of 8 wt % potassium hydroxide aqueous solution. The obtained solid was dissolved in boiling water, and the insoluble matter was removed by hot filtration. At 70° C., adjust the pH of the solution to ≤6 with 18% wt hydrochloric acid. The resulting white solid was filtered and recrystallized from ethanol to give white crystals. The yield is 58%.

[0090] The structural detection data of this compound are as follows (the proton nuclear magnetic spec...

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Abstract

The invention discloses an epoxy resin and a preparation method and application thereof. By introducing diphenyl ether and meta-position structure in the epoxy resin, when the viscosity of the epoxy resin is above the melting point of 65 DEG C, the epoxy resin can be abruptly reduced to below 0.1Pa.s; and the epoxy resin can be applied in the fields of encapsulation materials of integrated circuits, carbon fiber reinforced composite materials, adhesive, laminated boards and the like. The epoxy resin provided by the invention has the advantages of low processing viscosity, excellent heat resistance and the like, also has the advantages of low water absorption, low dielectric constant and low dielectric loss when being used for the encapsulation materials of the integrated circuits, and has important application value.

Description

technical field [0001] The invention belongs to the field of high-performance epoxy resins, and relates to an epoxy resin and its preparation method and application. Background technique [0002] In recent years, crystalline epoxy resin, as a kind of special epoxy resin, has a wide application prospect in modern industry due to its advantages of high purity, low melt viscosity above melting point, good fluidity, and high filling content of inorganic fillers. Usually, in the molecular structure of epoxy resin, the packing of molecular chains is relatively loose, so it is difficult to crystallize. However, the introduction of rigid symmetrical groups into the molecular structure of epoxy resins, such as biphenyl, often induces its crystallization. US Patent No. 4,072,656 reports a crystalline epoxy based on 3,3',5,5'-tetramethyl-4,4'-dihydroxybiphenyl (TMBP). TMBP reacts with epichlorohydrin, and by controlling the molar ratio of reactants and reaction conditions, crystallin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/295C07C41/26C07D303/30C07D301/28C08G59/24C08L63/02C09J163/02
Inventor 杨士勇宋涛封其立沈登雄陶志强刘金刚
Owner INST OF CHEM CHINESE ACAD OF SCI
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