含脂肪链的聚酰亚胺单体对称醚二胺的合成

Synthesis of polyimide symmetric monomer containing aliphatic ether diamine chain

摘要:

以对氯硝基苯和脂肪二醇为原料，在无水碳酸钾作用下经缩合和Pd/C催化氢化还原得到4个对称型聚酰亚胺二胺单体。以1,2-二（对氨基苯氧基）乙烷为例，考察了物料配比、碳酸钾用量、反应压力、催化剂用量等因素对收率的影响，得到了缩合反应较佳工艺条件为：乙二醇和对氯硝基苯的摩尔比为1:2.5，碳酸钾用量为15.9 g，反应时长24 h；还原反应的较佳工艺条件为：压力为0.6 MPa,催化剂用量为0.30 g，温度70 ℃。在该条件下，1,2-二（对氨基苯氧基）乙烷两步总收率为74.1%，其余3个二胺单体的合成收率在49.4%~65.7%。

Abstract:

A series of symmetric monomer of polyimide were prepared by condensation reaction and reduction reaction from p-chloronitrobenzene and the diols. The effects of the molar ratio of the materials, the amount of potassium carbonate, reaction time, reaction pressure and catalyst on the yield were studied. The optimum reaction conditions were obtained as follows: the molar ratio of raw materials1:2.5, the amount of potassium carbonate 15.9 g, reaction time 24 h；the reduction reaction pressure 0.6 MPa, the amount of catalyst 0.30 g, reaction temperature 70℃. The total yield of 1,2-bis (p-aminophenoxy) ethane was 74.1% under these condtions. The optimum reaction conditions were also applied in the synthesis of other 3 diamines with yields in the range of 49.4%~65.7%.