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以A(1,2-碳硼烷)为原料,分别采用琼斯试剂氧化法、CO2法和ClCOOCH3(氯甲酸甲酯)法合成了D(1,2-二羧基碳硼烷);然后D和B(1,2-二羟甲基碳硼烷)进一步酯化缩聚后,成功合成了P6(聚1,2-二羧基碳硼烷-1,2-二羟甲基碳硼烷酯)。研究结果表明:3种合成方法均能成功合成D,其中CO2法是最理想的合成方法;碳硼烷基团的引入,有效提高了P6的耐热性能(N2气氛中P6失重5%时的热解温度为190℃,700℃时的残炭率为59%);P6在耐高温领域中具有良好的应用前景,也是制备耐高温型PU(聚氨酯)胶粘剂的宝贵原材料。
D (1,2-dicarboxyborane) was synthesized from A (1,2-carborane) by Jones reagent oxidation, CO2 and ClCOOCH3 (methyl chloroformate) After further esterification polycondensation of B (1,2-dimethylol carborane), P6 (poly 1,2-dicarboxy carborane-1,2-dimethylol carborane ester) was successfully synthesized. The results showed that all the three synthetic methods could successfully synthesize D, of which CO2 was the best synthesis method. The introduction of carborane groups effectively enhanced the heat resistance of P6 (5% weight loss of P6 in N2 atmosphere The pyrolysis temperature is 190 ℃ and the carbon residue rate is 59% at 700 ℃). P6 has good application prospects in the field of high temperature and is also a valuable raw material for preparing high temperature resistant PU (polyurethane) adhesive.