甲基膦酸二甲酯的合成

Synthesis of dimethyl methylphosphonate

甲基膦酸二甲酯是一种添加型有机磷系阻燃剂,具有含磷量高、阻燃性能优异、价格低廉和添加量少等优点。以亚磷酸三甲酯为原料,对甲基苯磺酸甲酯为催化剂,通过重排反应合成甲基膦酸二甲酯。结果表明,在催化剂用量为亚磷酸三甲酯质量的8%、反应温度180℃和反应时间6 h条件下,产品收率约96%,催化剂可重复使用20次。气相色谱分析表明,亚磷酸三甲酯转化率为100%,甲基膦酸二甲酯粗品纯度大于99%,提纯后甲基膦酸二甲酯产品纯度大于99.7%。

Dimethyl methylphosphonate（ DMMP） is a kind of adding organic phosphorous flame retardants,and had the advantages of high phosphorus content,excellent flame retardant performance,low price and small addition quantity. Using trimethyl phosphite as the raw materials and methyl p-toluene sulfonic acid as the catalyst,dimethyl methylphosphonate was synthesized through rearrangement reaction. The results showed that the product yield of about 96% was obtained under the reaction condition as follows： catalyst dosage 8% of trimethyl phosphite mass,reaction temperature 180 ℃ and reaction time 6 h,and the catalyst could be reused 20 times. The results of gas chromatography analysis showed that the conversion rate of trimethyl phosphite was 100%,DMMP crude product purity was more than 99%,and after being purified,the purity of product DMMP was more than 99. 7%.