Bisphenol A novolac epoxy resin and preparation method thereof
A technology of novolac epoxy resin and phenolic resin, which is applied in the field of bisphenol A novolac epoxy resin and its preparation, can solve the problems of poor liquid separation and affecting the cycle, reduce side reactions, increase yield, and reduce process time Effect
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[0048] The bisphenol A formaldehyde epoxy resin provided by the invention has relatively low hydrolyzable chlorine content, less side reactions in the preparation method, clear interface during liquid separation, and reduced production cycle. Specifically, the invention discloses a preparation method of bisphenol A novolac epoxy resin, comprising the following steps:
[0049] A) Under anaerobic conditions, bisphenol A phenolic resin, epichlorohydrin, cosolvent, reducing agent and phase transfer catalyst are heated for reaction, and the intermediate is obtained by addition and ring opening to obtain a chlorohydrin ether structure;
[0050] B) The intermediate of the chlorohydrin ether structure obtained in the above step A) is subjected to a ring-closure reaction under the action of a basic catalyst, wherein, according to the amount of alkali added, the hydrolyzed chlorine of the resin in the product is controlled to be 2000 to 10000 ppm; during the reaction, the Water is disch...
Embodiment 1
[0082] First put 150g bisphenol A phenolic resin (SH-2130 type, Shandong Shengquan product), 700g epichlorohydrin, 70g isopropanol, 70g propylene glycol methyl ether, and 1g zinc powder into a 2L reaction bottle, at room temperature Stir for 30min. Then the reaction bottle was evacuated to a vacuum degree of 30KPa, and high-purity nitrogen gas was passed into the reaction bottle to replace the remaining air, and the operation was repeated twice. Finally, high-purity nitrogen was introduced to normal pressure, 10 g of benzyltriethylammonium chloride was added, and the reaction bottle was heated to 70° C., and after 4 hours of reaction, an intermediate with a chlorohydrin ether structure was obtained.
[0083]Then the reaction flask is evacuated, and the vacuum degree is 23KPa, and it is refluxed under reduced pressure at 69°C, and 84.17g of NaOH solution with a mass concentration of 47.5% is added dropwise to the intermediate of the chlorohydrin ether structure in the reaction ...
Embodiment 2
[0087] First put 150g bisphenol A phenolic resin (SH-2130 type, Shandong Shengquan product), 900g epichlorohydrin, 180g isopropanol, 90g propylene glycol methyl ether and 1g zinc powder into a 2L reaction bottle, stir at room temperature 30min. Then the reaction bottle was evacuated to a vacuum degree of 30KPa, and high-purity nitrogen gas was passed into the reaction bottle to replace the remaining air, and the operation was repeated twice. Finally, high-purity nitrogen was introduced to normal pressure, 6g of tetraethylammonium chloride was added, and the reaction bottle was heated to 70°C. After 4 hours of reaction, an intermediate with a chlorohydrin ether structure was obtained.
[0088] Then the reaction flask is evacuated, and the vacuum degree is 25KPa, and it is refluxed under reduced pressure at 68°C, and 80.5g of mass concentration is added dropwise to the intermediate of the chlorohydrin ether structure in the reaction flask, and the NaOH solution is 47.5%, using a...
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Abstract
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