有机过氧化物交联剂二(叔丁基过氧化异丙基)苯的合成研究

Study on the Synthesis of Organic Peroxide Crosslinking Agent Di(tert butylperoxide isopropyl)Benzene

以叔丁基过氧化氢(TBHP)、α,α’-二羟基-1,3-二异丙基苯(Diol)为反应原料,以乙酸酐为脱水剂脱去70%TBHP中的水,以乙酸酐与水反应后生成的乙酸为催化剂合成二(叔丁基过氧化异丙基)苯(BIBP)。研究了物料配比、反应温度、反应时间、干燥温度、干燥压力和干燥时间对合成交联剂BIBP的影响,得到了最佳反应条件:反应温度50℃、反应时间30 min、TBHP/乙酸酐的质量比为1/2、TBHP/Diol物质的量比为2.2/1、真空闪蒸干燥温度为50℃、压力为–0.095MPa、时间1h。该合成条件下所得到的BIBP产品呈纯白色固体,纯度为98.930%,收率为91.85%。

Using tert-butyl hydroperoxide(TBHP)andα,α'-dihydroxy-1,3-diisopropylbenzene(Diol)as the reaction material,and acetic anhydride was used as dehydrating agent to remove water from 70%TBHP.The acetic acid generated after the reaction of acetic anhydride with water was used as the catalyst to synthesize bis(tert butyl peroxyisopropyl)benzene(BIBP).The effects of material ratio,reaction temperature,reaction time,drying temperature,drying pressure,and drying time on the synthesis of crosslinking agent BIBP were studied.The optimal reaction conditions were as follows:the reaction temperature was 50℃,the reaction time was 30 min,the mass ratio of TBHP/acetic anhydride was 1/2,the molar ratio of TBHP/Diol material was 2.2/1,the vacuum flash drying temperature was 50℃,the pressure was–0.095 MPa,and the time was 1 h.Under the synthetic conditions,the BIBP product was a pure white solid with a purity of 98.930%and a yield of 91.85%.