磷酸二-(2,3-二氯丙基)六次甲胺盐阻燃剂的合成

Synthesis of Di-(2,3-dichloropropyl) Phosphate of Hexamethylene Tetramine

以环氧氯丙烷、三氯氧磷、六次甲基四胺(HT)为原料,以AlCl3为催化剂,先合成磷酸双(2,3二氯丙基)酯(DP),再合成一种新型含氮、磷和氯的阻燃剂———磷酸二-(2,3-二氯丙基)六次甲基四胺盐(DPHT),研究了反应物配比、反应温度、反应时间等对中间体DP和最终产物DPHT产率的影响。结果表明,中间体DP的最佳合成条件为:nECH∶nPOC=2∶1,催化剂AlCl3最佳用量约为环氧氯丙烷的2%,反应温度为333～343K,反应时间为1.5～2h;产物DPHT的最适宜合成条件为:nDP∶nHT=1∶2,反应温度为323～333K,反应时间为2h。

A new type of retardant-di-(2,3-di-chloropropyl) phosphate of hexamethy lenamine (DPHT)containing nitrogen, phosphorus and chlorine was synthesized using hexamethy lenamine(HT), epichlorohydrin(ECH), phosphorus oxychloride(POC). AlCl3 was used as catalyst. Di-(2,3-di-chloropropyl) phosphate(DP) was synthesized firstly. The effects of the molar ratio, reaction temperature and the like on the yield of DP and DPHT were investigated. Result showed that, the optimal condition of DP reaction was that nECH : nPOC=2:1, the concentration of AlCl3 was 2% of ECH, the reaction temperature was about 333～343 K and the reaction time was about 1.5～2h; the optimal condition of DPHT reaction was that nDP: nHT=1:2, reaction temperature was about 323～333 K, and the reaction time was about 2h.