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Preparation method of high-Tg halogen-free flame retardant epoxy resin

A technology of epoxy resin and compound, which is applied in the field of preparation of high Tg halogen-free flame retardant epoxy resin, can solve the problems that cannot meet the high heat resistance requirements of lead-free soldering, reduce the electrical insulation performance of materials, and affect the service life of electrical appliances, etc. , to achieve the effects of easy operation, high resin-glass transition temperature, and high cross-linking density

Active Publication Date: 2015-02-18
JINAN SHENGQUAN GROUP SHARE HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, brominated epoxy resins were widely used in copper clad laminates and packaging materials due to their excellent flame retardancy and physical and mechanical properties. However, brominated epoxy resins are easily hydrolyzed to produce HBr when used, which reduces the electrical insulation properties of the material. And it has been proved that carcinogens such as polybrominated dibenzodioxin (PBDD) and polybrominated dibenzofuran (PBDF) are produced during the combustion process, which has been banned by relevant laws and regulations of the European Union and China
In addition, when the copper clad laminate is used under high temperature conditions, halogen elements such as bromine are easily dissociated, which affects the service life of electrical appliances
[0003] Patent document CN1737056A discloses a phosphorus-containing epoxy resin composition and its application. The phosphorus-containing epoxy resin is obtained by reacting a phosphorus-containing organic compound with an epoxy resin. However, the phosphorus-containing epoxy resin obtained by this method After the resin is cured, the Tg (glass transition temperature) is around 130°C, which is far from meeting the high heat resistance requirements of lead-free soldering today.

Method used

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  • Preparation method of high-Tg halogen-free flame retardant epoxy resin
  • Preparation method of high-Tg halogen-free flame retardant epoxy resin
  • Preparation method of high-Tg halogen-free flame retardant epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 2000ml four-necked flask, add 68g of 1,4-naphthoquinone, 352g of DOPO, add 827g of xylene, under the protection of nitrogen, heat and stir to dissolve, when the temperature rises to 110°C, react at constant temperature for 4h; Bisphenol A formaldehyde epoxy resin SQAN-201 (Shandong Shengquan Chemical Co., Ltd. product, EEW 193g / eq) 1120g, bisphenol A epoxy resin SQE-901 (Shandong Shengquan Chemical Co., Ltd. product, EEW 465g / eq ) 29g, trifunctional epoxy resin SQSN-331 (product of Shandong Shengquan Chemical Co., Ltd., EEW168g / eq) 39g, heating up to 170°C, adding catalyst triphenylphosphine 0.71g, keeping the temperature at 170°C for 5h, to obtain ring oxygen resin. After testing, the epoxy equivalent is 423g / eq, and the phosphorus content is 3.1%.

Embodiment 2

[0020] In a 2000ml four-neck flask, add 1,4-benzoquinone 79.8g, DOPO 235.1g, add toluene 821g, under the protection of nitrogen, heat and stir to dissolve, when the temperature rises to 115°C, react at constant temperature for 3h; Add bisphenol A formaldehyde epoxy resin SQAN-203 (Shandong Shengquan Chemical Co., Ltd. product, EEW200geq) 1180g, four functional epoxy resin SQE-431 (Shandong Shengquan Chemical Co., Ltd. product, EEW216g / eq) 58g, heating The temperature was raised to 165°C, 0.74 g of triethylphosphine was added as a catalyst, and the temperature was kept at 165°C for 4 hours to obtain an epoxy resin. After testing, the epoxy equivalent is 378g / eq, and the phosphorus content is 2.1%.

Embodiment 3

[0022] In a 2000ml four-necked flask, add 37g of 1,4-naphthoquinone, 196g of DOPO, and 834g of butanone, under the protection of nitrogen, heat and stir to dissolve. Phenol novolac epoxy resin SQPN-638 (Shandong Shengquan Chemical Co., Ltd. product, EEW175g / eq) 769g, add bisphenol A epoxy resin SQE-901 (Shandong Shengquan Chemical Co., Ltd. product, EEW 465g / eq) 87g , 473g of trifunctional epoxy resin SQSN-331 (product of Shandong Shengquan Chemical Co., Ltd., EEW168g / eq), heated to 180°C, added 0.76g of catalyst triphenylphosphine, and kept at 180°C for 3h to obtain epoxy resin . After testing, the epoxy equivalent is 417g / eq, and the phosphorus content is 1.8%.

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Abstract

The invention provides a preparation method of high-Tg halogen-free flame retardant epoxy resin and belongs to the technical field of epoxy resin. The preparation method comprises the following steps: S1) adding a quinone compound and a phosphorous compound into a certain solvent and raising the temperature under nitrogen protection to react so as to obtain a phosphorous intermediate; and S2) removing the solvent under reduced pressure, then adding multifunctional epoxy resin and a catalyst, and continuously raising the temperature to react so as to prepare the high-Tg halogen-free flame retardant epoxy resin. Compared with the prior art, the method has the advantages that the prepared halogen-free flame retardant epoxy resin prepared has Tg being over 170 DEG C and is free of halogen, so that the heat resistance of the resin is improved. The flame retardant property of the resin can reach the level UL94V-0, so that the requirement that a copper-clad plate is halogen-free and highly heat-resistant is satisfied. Moreover, when the copper-clad plate is combusted, no toxic gas is generated, so that the requirement for environmental protection is satisfied. In addition, the preparation method is simple in process, convenient to operate and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of epoxy resin, in particular to a preparation method of high Tg halogen-free flame-retardant epoxy resin. Background technique [0002] With the deepening of the lead-free soldering era, in order to comply with the requirements of environmental protection, it is imminent for copper clad laminate manufacturers to develop a high glass transition temperature, halogen-free, flame-retardant copper clad laminate substrate. On July 1, 2006, the RoHS environmental protection directive issued by the European Union was officially implemented, and it also marked that the global electronics industry has entered the era of lead-free soldering. The temperature of lead-free soldering is 20°C higher than that of traditional lead-based soldering, which puts forward higher requirements for the heat resistance and reliability of the printed circuit board substrate, and also requires good flame retardancy. In the past, bromin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/20C08G59/38C08G59/40
Inventor 江成真朱红军葛成利刘萌
Owner JINAN SHENGQUAN GROUP SHARE HLDG