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Fluorine-containing epoxy resin and preparation method thereof

An epoxy resin and glycidyl technology, applied in the direction of organic chemistry, etc., can solve the problems of easy contamination of the surface of the cured product, high surface energy of epoxy resin, limited application of epoxy resin, etc., and achieves high glass transition temperature, The effect of strong hydrophobicity and low water absorption

Inactive Publication Date: 2013-10-23
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the high surface energy of epoxy resin makes the surface of the cured product easy to pollute; the large number of hydroxyl groups in the molecular structure increases the moisture absorption rate of the material, which greatly limits the application of epoxy resin in coatings for ships and large structural parts

Method used

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  • Fluorine-containing epoxy resin and preparation method thereof
  • Fluorine-containing epoxy resin and preparation method thereof
  • Fluorine-containing epoxy resin and preparation method thereof

Examples

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preparation example Construction

[0022] The following examples are the preparation method of fluorine-containing epoxy resin and the properties of its cured product are attached to illustrate the excellent performance of the fluorine-containing epoxy resin after curing.

[0023] Characterization and test methods: Infrared spectrum is measured by Perkin-Elmer 782 Fourier transform infrared spectrometer, the sample preparation method is KBr tablet method or thin film method, and the measuring range is 4000~400cm -1 . The electrical properties were tested using a Hewlett-Packard 4284A Presion LCR tester. The dielectric constant and dielectric loss are measured by LKI-1 capacitance meter, the temperature is 25°C, and the frequency is 1MHz. Dynamic mechanical analysis (DMA) test adopts the Q-800 type instrument measurement of American TA company, glass transition temperature (T g ) is represented by the temperature corresponding to the peak of the loss tangent (tanδ).

Embodiment 1

[0025] 1,1-bis[3-methyl-4-(2,3-epoxypropyl)phenyl]-1-(2',3',4',5',6'-pentafluorophenyl) -2,2,2-Trifluoroethane

[0026] At room temperature, 132 grams of 2-methylphenol, 10 grams of trifluoromethanesulfonic acid and 66 grams of 2,3,4,5,6-pentafluoro-α, α, α-trifluoroacetophenone in a 250ml reaction bottle Mix evenly, heat to 50°C and stir for about 1 hour to completely dissolve 2-methylphenol to form a homogeneous liquid. Raise the temperature to 120°C and stir, carry out the condensation reaction under the catalysis of trifluoroacetic acid for 6 to 8 hours, and obtain a brownish-red liquid, which is distilled under reduced pressure to remove excess 2-methylphenol, and the crude product is dissolved in ethanol and water (ethanol: the volume of water Recrystallization was carried out in a mixed solution with a ratio of 1:1), and 98.175 g of white solid was obtained, with a yield of 85%.

[0027] 100 grams of the above white solid and 400 grams of epichlorohydrin were stirred ...

Embodiment 2

[0031] 1,1-bis[3,5-dimethyl-4-(2,3-epoxypropyl)phenyl]-1-(2',3',4',5',6'-pentafluoro Phenyl)-2,2,2-trifluoroethane

[0032]At room temperature, 90 grams of 2,6-dimethylphenol, 5 grams of trifluoromethanesulfonic acid and 48 grams of 2,3,4,5,6-pentafluoro-α, α, α-trifluoroacetophenone in 250ml After mixing evenly in the reaction flask, heat to 50°C and stir for about 1 hour to completely dissolve 2,6-dimethylphenol to form a homogeneous liquid. Warm up to 120°C and stir, and condense under the catalysis of trifluoromethanesulfonic acid for 12 hours to obtain a brownish-red liquid, which is distilled off under reduced pressure to remove excess 2,6-xylenol, and the crude product is dissolved in ethanol and water (ethanol: water Recrystallization was carried out in the mixed solution whose volume ratio was 4:1), and 71 g of white solid was obtained, and the yield was 80%.

[0033] Stir and mix 100 grams of the above-mentioned white solid with 800 grams of epichlorohydrin, add 65...

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Abstract

The invention relates to epoxy resin, and in particular relates to fluorine-containing epoxy resin and a preparation method thereof. The method comprises the following steps of: performing a condensation reaction on a substituted alpha, alpha, alpha-trifluoro-multifluoro-substituted phenyl ethyl ketone and 2-methylphenol (or 2,6-xylenol) under the catalysis of a lewis acid, thereby preparing a fluorine-containing diphenol compound; and then performing a reaction on the fluorine-containing diphenol compound and epoxy chloropropane under the catalysis of an alkali, thereby obtaining the fluorine-containing epoxy resin having the structure in the following formula. The fluorine-containing epoxy resin is cured by using a commonly-used epoxy resin curing agent, so that the cured fluorine-containing epoxy resin has the advantages of high vitrifaction transformation temperature, excellent electrical property, low water absorption rate, strong hydrophobicity and the like. Thus, the fluorine-containing epoxy resin can be possibly applied to the fields of microelectronic packaging and surface coating.

Description

technical field [0001] The invention relates to epoxy resins, in particular to a fluorine-containing epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resins are widely used in coatings, adhesives, electronics, civil engineering, composite materials and other fields due to their strong adhesion, excellent electrical insulation, stable chemical properties, and excellent processability. High-performance epoxy resin with special structure, as an important packaging material for microelectronic devices, including epoxy molding compound, conductive silver paste, etc., has a very important position and role in the field of microelectronic packaging. With the development of microelectronic devices in the direction of short, small, light and thin, higher and higher requirements are put forward for epoxy resin, mainly including: 1) high heat resistance, 2) low water absorption, 3) low dielectric Electrical constant and dielectric loss, 4) low stress, ...

Claims

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Application Information

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IPC IPC(8): C07D303/27C07D301/28
Inventor 尚呈元黄伟赵晓娟杨欣张英
Owner INST OF CHEM CHINESE ACAD OF SCI
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