CAJ | 학술논문

利用双酚A结晶残液为原料,以磺化聚氯代苯乙烯-二乙烯基苯强酸性阳离子交换树脂为催化剂,通过固定床连续催化制备6,6’-二羟基-3,3,3’,3’-四甲基-1,1’-螺二氢茚。反应器中装填50mL（22 g,E=1.8 mmol H＋/mL）干树脂,在T=150℃、WHVS=0.48 h-1条件下,连续反应1000 h,反应液中6,6’-二羟基-3,3,3’,3’-四甲基-1,1’-螺二氢茚质量浓度可达43.5%,催化剂交换量保持为3.8 mmol/g。产物经重结晶纯化后熔点215～217℃,纯度≥99.98%（HPLC）。通过HPLC、IR、NMR等方法分析产物含量及结构,用STATISTIC统计软件对反应条件进行了优化。研究结果对于改进双酚A生产工艺中的残液处理方式,填补国内在新型双酚类单体生产空白具有重要的意义。
이용쌍분A결정잔액위원료,이광화취록대분을희-이을희기분강산성양리자교환수지위최화제,통과고정상련속최화제비6,6’-이간기-3,3,3’,3’-사갑기-1,1’-라이경인。반응기중장전50mL（22 g,E=1.8 mmol H＋/mL）간수지,재T=150℃、WHVS=0.48 h-1조건하,련속반응1000 h,반응액중6,6’-이간기-3,3,3’,3’-사갑기-1,1’-라이경인질량농도가체43.5%,최화제교환량보지위3.8 mmol/g。산물경중결정순화후용점215～217℃,순도≥99.98%（HPLC）。통과HPLC、IR、NMR등방법분석산물함량급결구,용STATISTIC통계연건대반응조건진행료우화。연구결과대우개진쌍분A생산공예중적잔액처리방식,전보국내재신형쌍분류단체생산공백구유중요적의의。
In this paper,a new preparation method of a continuous fixed-bed catalytic system for 6,6’-dihydroxy-3,3,3’,3’-tetramethyl-1,1’-spirobiindane was reported with bisphenol A crystalline residue solution as raw material,and sulfonated polyvinyl generation of styrene-divinylbenzene strong acid cation exchange resin as catalyst.Stainless steel reactor with ？30 mm was filled by 50 mL（22g,E = 1.8 mmol H＋/mL） dry resin.In the condition of T =150 ℃,WHVS = 0.48h-1,it had reacted continuously for 1000 h,the concentration of 6,6 ’-dihydroxy-3,3,3’,3’-tetramethyl-1,1’-spirobiindane in reaction solution was stabilized at 43.5%,and the exchange capacity of catalyst remained 3.8 mmol/g.Product was purified by recrystallization,and the melting point was 215—217 ℃,purity was≥ 99.98%（HPLC）.By HPLC,IR,NMR and other methods for the analysis of product content and structure,reaction conditions were optimized with a statistical software STATISTIC.The results for the improvement on the production process of bisphenol A residue treatment suggest a brand new method for bisphenol monomer production.