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Hybrid organic silicon-phosphorus type epoxy modifying agent used for copper clad laminate of printed circuit board, preparation method and application thereof

A technology of organosilicon and modifier, which is applied in the field of hybrid organosilicon-phosphorus epoxy modifier and its preparation, can solve the problems of brittleness, decreased heat resistance, poor heat resistance, etc., and achieve modification The effect of simple process, improved heat resistance, and strong practicability

Inactive Publication Date: 2009-10-14
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, domestic and foreign copper-clad laminate products basically use epoxy resin as the matrix resin. However, due to the high cross-linking structure of pure epoxy resin, there are disadvantages such as brittleness, fatigue, poor heat resistance, and poor impact toughness. Therefore, Difficult to be directly used as a base material for new printed circuit copper clad laminates
In addition, epoxy resin is flammable. At present, bromine-containing epoxy resin is widely used in flame retardant technology, but it will release toxic gases such as hydrogen bromide and diphenyl dioxin during combustion, which is harmful to the environment and human body.
[0003] Scholars at home and abroad generally adopt the method of blending or graft copolymerization to modify epoxy resin with silicone, but it is difficult to toughen and improve heat resistance at the same time, or increase toughness but decrease heat resistance, or Increased heat resistance but reduced toughness
In terms of flame retardant performance improvement, some scholars introduce phosphorus into epoxy resin to achieve flame retardant effect, but it reduces the heat resistance of epoxy resin
Therefore, how to improve the heat resistance, toughness and flame retardancy of epoxy resin at the same time to meet the requirements of advanced copper clad laminates is still a difficult problem at home and abroad.

Method used

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  • Hybrid organic silicon-phosphorus type epoxy modifying agent used for copper clad laminate of printed circuit board, preparation method and application thereof
  • Hybrid organic silicon-phosphorus type epoxy modifying agent used for copper clad laminate of printed circuit board, preparation method and application thereof
  • Hybrid organic silicon-phosphorus type epoxy modifying agent used for copper clad laminate of printed circuit board, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 236g of glycidoxypropyltrimethylsilane, 138g of diethyl phosphite, and 2g of triphenylphosphine into a three-necked flask, stir it electrically, reflux at 150°C for 3h, and then cool to prepare a phosphorus-containing active agent.

[0037] Take another 200g of methyltriethoxysilane, 20g of deionized water, and 0.5g of dibutyltin dilaurate, stir, reflux and hydrolyze at 80°C for 8 hours, and remove small molecules of water after the reaction to obtain polymethyltriethyl triethyl Oxysilane.

[0038] Add 475g of phosphorus-containing active agent, 105g of polymethyltriethoxysilane, 18g of deionized water, and 2g of dibutyltin dilaurate into the reactor in sequence, stir, and reflux at 100°C for 6h, and cool to obtain the hybrid organic Silicon phosphorus epoxy modifier.

[0039] Take 100g of bisphenol A epoxy resin (E54) with an epoxy value of 0.54mol / g, add 25g of the above-mentioned modifier, stir evenly, and then vacuumize in a vacuum oven at 80°C for 1h, then add...

Embodiment 2

[0041]Add 22 g of methyl (γ-glycidoxy) diethoxysilane, 14 g of dimethyl phosphate, and 0.2 g of triethylamine into a three-necked flask, stir it electrically, and reflux at 120°C for 6 hours to obtain a phosphorus-containing Active agent; then add 10 g of commercially available polymethyltrimethoxysilane, 0.5 g of deionized water, and 0.2 g of tin tetrachloride, continue to stir, and reflux at 60 ° C for 8 hours, and cool to obtain a hybrid organosilicon phosphorus ring Oxygen modifier.

[0042] Take 10g of novolac epoxy with an epoxy value of 0.48mol / g, add 2.5g of the above-mentioned modifier, then add 6.3g of novolak resin and 0.2g of triphenylphosphine, stir well and vacuumize at 60°C for 2h, then Inject into the mold, keep the vacuum, 1h at 90°C, 2h at 150°C, 3h at 200°C. The Tg of the obtained epoxy cured product is 172.50°C, the limiting oxygen index (LOI) is 24.3, and the tensile strength is 51.93 MPa.

Embodiment 3

[0044] Glycidoxypropyltriethylsilane 260g, 10-oxygen-(9,10-2H-9-oxo-10phospho)phenanthrene (DOPO) 216g, ethyl triphenylphosphonium ester / acetate complex Add 3g of the compound into a three-necked flask, stir electrically, and reflux at 130°C for 5h to obtain a phosphorus-containing active agent; cool, then add 50g of commercially available polymethyltriethoxysilane, 10g of deionized water, and 2g of stannous octoate , continue to stir, and reflux at 80 ° C for 4 hours, and cool to obtain a hybrid organic silicon phosphorus epoxy modifier.

[0045] Get 100g of bisphenol A epoxy resin (E51) with an epoxy value of 0.51mol / g, add 25g of the above-mentioned modifier, add 83g of novolac resin, 0.05g of 2-ethyl-4-methylimidazole, and stir evenly Then vacuumize at 80°C for 2h, then inject into the mold, keep the vacuum, 120°C for 3h, 220°C for 3h. The Tg of the obtained epoxy cured product is 155.88°C, the limiting oxygen index (LOI) is 24.9, and the tensile strength is 71.36MPa.

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Abstract

The invention discloses a hybridized organic silicon-phosphorus type epoxy modifying agent used for a copper clad laminate of a printed circuit board, a preparation method and application thereof. The hybrid organic silicon-phosphorus type epoxy modifying agent is prepared by the following steps: mixing and stirring 100-500 parts of phosphoric active agents, 10-300 parts of polysiloxanes, 0.05-5 parts of catalysts and 0.1-20 parts of deionized water based on parts by weight, carrying out reflux and hybridization on the mixture at the temperature of 60-120 DEG C for 2-8h and then cooling the mixture. The hybridized organic silicon-phosphorus type epoxy modifying agent is applied to epoxy resins used for modifying the copper clad laminate of the printed circuit board.

Description

technical field [0001] The invention relates to the field of epoxy resins, in particular to a hybrid organo-silicon-phosphorus epoxy modifier for printed circuit copper-clad laminates and a preparation method and application thereof. Background technique [0002] Epoxy resin has the advantages of excellent mechanical properties, electrical properties, chemical properties, adhesive properties, easy molding and processing, and low cost. It is widely used in the matrix of coatings, adhesives, electrical and electronic insulation, and advanced composite materials. At present, domestic and foreign copper-clad laminate products basically use epoxy resin as the matrix resin. However, due to the high cross-linking structure of pure epoxy resin, there are disadvantages such as brittleness, fatigue, poor heat resistance, and poor impact toughness. Therefore, It is difficult to directly use it as a base material for new printed circuit copper clad laminates. In addition, epoxy resin i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/14C08G77/30C08G59/14C08L63/00
Inventor 刘伟区胡朝辉
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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