摘要
以烯丙醇为起始剂 ,先合成了α 烯丙基齐聚氧化乙烯 氧化丙烯单醇 ;再加入甲醇钠溶液使聚醚的羟基转化为醇钠基团 ;加入一氯甲烷进行封端反应 ,经精制 ,得到α 烯丙基齐聚氧化乙烯 氧化丙烯甲醚。考察了聚醚合成时反应温度、KOH用量对聚醚羟值的影响 ,尤其研究了聚醚羟基封端工艺中反应条件对产品质量的影响。实验表明采用旋转薄膜蒸发器进行封端反应 ,封端效率高。制备设计相对分子质量为 30 0 0的烯丙基齐聚醚 ,得到的聚醚羟值为 2 2 .3mgKOH/g。当羟基 /甲醇钠 /一氯甲烷摩尔比为 1∶2∶2 .5 ,110℃真空脱甲醇 1h ,加入一氯甲烷后在 80℃反应 1h ,封端率可达 90 %以上。所得低聚物主要用于非水解型 (SiC型 )
allyl poly(oxyethylene oxypropylene) monol was firstly synthesized with allyl alcohol as initiator, then sodium methoxide methanol is added to convert the hydroxyl to sodium alcoholate group, methane chloride was added to carry out the methoxyl capping reaction, α allyl poly(oxyethylene oxypropylene) methyl ether was obtained by purifying. The effects of reaction temperature and KOH dosage on the hydroxyl value of the oligomer monol, the effect of reaction condition on the polyether methyl ether were investigated. The results show that, if the revolving film evaporator is adopted, the capping efficiency is elevated. The polyether with hydroxyl value 22.3 mgKOH/g was acquired when the design molecular weight is 3000. When the molar ratio of hydroxyl/sodium methoxide/methane chloride is 1/2/2.5, and removing methanol 1 hour under 110℃ & reduced pressure, reacting 1 hour at 80℃after adding of methane chloride, the methoxyl capping rate reach over 90%. The prepared oligomer is mainly used in the synthesis of non hydrolyzable foam stabilizers for flexible polyurethane foams.
出处
《聚氨酯工业》
2002年第1期15-18,共4页
Polyurethane Industry