三甘醇用于液晶聚酯聚合反应釜的洗釜工艺研究

Study of the Washing Technology of Polymerizing-kettle for Liquid Crystal Polyester by Triethylene Glycol

以4-羟基苯甲酸/6-羟基-2-萘甲酸(73/27)组成的液晶聚合物聚合反应釜的清洗工艺为研究对象,聚合反应结束出料后,采用三甘醇/氢氧化钠为洗釜液对反应釜进行清洗,系统研究了洗釜的条件。结合气相色谱-质谱分析,考察了氢氧化钠含量、洗釜温度、洗釜时间及三甘醇洗液回收重复洗釜等条件对洗釜效率的影响。研究结果表明:当氢氧化钠含量在6.9%时,洗釜温度在210℃以上时,洗釜时间在4 h以上,即可完成高效率的反应釜清洗,且三甘醇洗液可回收重复利用。

With the studying object of the cleaning technology of polymerizing-kettle with liquid crystal polyester consisting of 4-hydroxybenzoic acid/6-hydroxy-2-naphthoic acid （73/27）, the mixture of triethylene glycol/sodium hydroxide was used to clean the polymerizing-kettle after discharging the polymer, and the washing conditions were studied systematically. Combined with the meteorological chromatography- mass spectrometry analysis, the effect of the solid content of sodium hydroxide, temperature, time and washing times of the recovery triethylene glycol on the cleaning efficiency were studied. The results show that： when the solids content of sodium hydroxide is 6.9%, the temperature is above 190℃ and the time is above 4 h, reactor cleaning is completed efficiently, and the mixture of triethylene glycol/sodium hydroxide can be reused.