Preparation method of tetramethyl bisphenol F epoxy resin

A technology of tetramethyl bisphenol and epoxy resin, applied in the field of epoxy resin, can solve the problems of high melting point and increased filling amount of filler, and achieve the effects of simple operation, increased production profit and reduced production cost

Inactive Publication Date: 2015-04-01
JINAN SHENGQUAN GROUP SHARE HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent document CN1733745A discloses a preparation method of 3,3',5,5'-tetramethyl-4,4'-biphenyl diglycidyl ether, the 3,3',5,5'-tetra Methyl-4,4'-biphenyl diglycidyl ether has a high melting point above 90°C, so in the application of semiconductor packaging materials, the filling amount of the epoxy resin still needs to be further improved

Method used

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  • Preparation method of tetramethyl bisphenol F epoxy resin
  • Preparation method of tetramethyl bisphenol F epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 140g of 4,4'-methylenebis(2,6-dimethyl)phenol, 690g of epichlorohydrin, and 2g of glycerol into a four-necked flask with stirring and a thermometer. Under the protection of nitrogen, , heat and stir to dissolve, add 25g of sodium bicarbonate solution with a mass fraction of 20%, and react at 60°C for 4 hours, then add 98g of 50% sodium hydroxide solution under a vacuum of 0.06MPa to catalyze the ring-closing reaction, react for 6h, and depressurize Recovery of epichlorohydrin. Then add 140g of toluene and 140g of cyclohexanone, add 8g of 50% sodium hydroxide solution for refining, react at 85°C for 3h, wash with water until neutral, and remove the solvent under reduced pressure to obtain tetramethylbisphenol F epoxy resin. Test results: melting point: 72°C, viscosity: 0.11p (150°C), epoxy equivalent: 195g / eq.

Embodiment 2

[0025] Add 140g of 4,4'-methylenebis(2,6-dimethyl)phenol, 750g of epichlorohydrin, and 8g of 1,4-dioxane into a four-neck flask with stirring and a thermometer. Under the protection of high-purity nitrogen, heat and stir to dissolve, add 50g of potassium hydroxide solution with a mass fraction of 10%, react at 40°C for 4 hours, add 110g of 50% potassium bicarbonate solution under vacuum of 0.07MPa to catalyze the ring-closing reaction, After 5 hours of reaction, epichlorohydrin was recovered under reduced pressure. Then add 258g of methyl isobutyl ketone, add 10g of sodium carbonate solution with a mass fraction of 50% to refine, react at 85°C for 3h, wash with water until neutral, and remove the solvent under reduced pressure to obtain tetramethylbisphenol F epoxy resin. Test results: melting point: 69°C, viscosity: 0.08p (150°C), epoxy equivalent: 193.5g / eq.

Embodiment 3

[0027] Add 140g of 4,4'-methylenebis(2,6-dimethyl)phenol, 520g of epichlorohydrin in a four-neck flask with stirring and a thermometer, add ethylene glycol dimethyl ether 4g, and Under the protection of pure nitrogen, heat and stir to dissolve, add 100g of sodium hydroxide solution with a mass fraction of 5%, and react at 60°C for 4 hours, then add 150g of 40% sodium hydroxide solution under a vacuum of 0.04MPa to catalyze the ring-closing reaction. After 5 hours of reaction, epichlorohydrin was recovered under reduced pressure. Then add 320g of cyclohexanone, add 10g of sodium bicarbonate solution with a mass fraction of 50% to refine, react at 60°C for 3h, wash with water until neutral, and remove the solvent under reduced pressure to obtain tetramethylbisphenol F epoxy resin. Test results: melting point: 69°C, viscosity: 0.08p (150°C), epoxy equivalent: 196.2g / eq.

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Abstract

The invention discloses a preparation method of a tetramethyl bisphenol F epoxy resin, belonging to the technical field of epoxy resins. The tetramethyl bisphenol F epoxy resin is prepared from 4,4'-methylene-bis(2,6-dimethyl)phenol and epoxy chloropropane in a mass ratio of 1:3-1:10. The preparation method comprises the following steps: (1) adding the 4,4'-methylene-bis(2,6-dimethyl)phenol and epoxy chloropropane, adding a cosolvent, adding an alkaline catalyst at 40-70 DEG C in a nitrogen protective atmosphere, reacting for 1-4 hours, adding an alkaline catalyst, reacting in a vacuum for 2-7 hours, and recovering the epoxy chloropropane under reduced pressure; and (2) adding a solvent and an alkaline catalyst, after the reaction finishes, washing with water to a neutral state, and removing the solvent to obtain the product. The tetramethyl bisphenol F epoxy resin obtained by the preparation method has lower melting point and viscosity, can implement high filling content in the semiconductor packaging material, and especially has favorable application prospects in the field of high-performance electronic packaging.

Description

technical field [0001] The invention relates to the technical field of epoxy resins, in particular to a preparation method of tetramethyl bisphenol F epoxy resin. Background technique [0002] Electronic packaging materials are base materials used to carry electronic components and their interconnections, and play the roles of mechanical support, sealing environment protection, signal transmission, heat dissipation and shielding. have a very important impact. With the vigorous development of microelectronics industry, microelectronic packaging technology has been developed rapidly, but the research on microelectronic packaging materials is relatively slow. At present, microelectronic products are developing in the direction of high integration, miniaturization of wiring, three-dimensional assembly, large-scale chip, green environmental protection, etc., which puts forward new requirements for microelectronic packaging materials, that is, to the high-tech electronic industry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
Inventor 祝建勋朱红军邓亚玲
Owner JINAN SHENGQUAN GROUP SHARE HLDG
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