盐城工学院学报:自然科学版
鹽城工學院學報:自然科學版
염성공학원학보:자연과학판
Journal of Yancheng Institute of Technology(Natural Science Edition)
2012年
1期
15-18,57
,共5页
缩水甘油基叔丁基醚%加成反应%环化作用%催化
縮水甘油基叔丁基醚%加成反應%環化作用%催化
축수감유기숙정기미%가성반응%배화작용%최화
tert-butyl glycidyl ether%additive reaction%cylic action%catalysis
以环氧氯丙烷(ECH)和叔丁醇(TBA)为原料,经加成反应和环化作用,合成了缩水甘油基叔丁基醚(TBGE);研究了催化剂类型、ECH与TBA物料比、催化剂用量、加成反应温度及时间等因素对TBGE收率的影响,用气相色谱法分析了产品中TBGE含量,GC-MS和FT-IR等表征了产物结构。实验结果表明,三氟化硼(BF3)-乙醚是性能优良的催化剂;在BF3-乙醚的用量为TBA质量的3.0%、加成反应的温度和时间分别为50.0℃和5.0 h、nECH/nTBA为2.5的条件下,TBGE的收率可达85%以上;气相色谱的分析结果表明产品中TBGE含量在99.0%以上。
以環氧氯丙烷(ECH)和叔丁醇(TBA)為原料,經加成反應和環化作用,閤成瞭縮水甘油基叔丁基醚(TBGE);研究瞭催化劑類型、ECH與TBA物料比、催化劑用量、加成反應溫度及時間等因素對TBGE收率的影響,用氣相色譜法分析瞭產品中TBGE含量,GC-MS和FT-IR等錶徵瞭產物結構。實驗結果錶明,三氟化硼(BF3)-乙醚是性能優良的催化劑;在BF3-乙醚的用量為TBA質量的3.0%、加成反應的溫度和時間分彆為50.0℃和5.0 h、nECH/nTBA為2.5的條件下,TBGE的收率可達85%以上;氣相色譜的分析結果錶明產品中TBGE含量在99.0%以上。
이배양록병완(ECH)화숙정순(TBA)위원료,경가성반응화배화작용,합성료축수감유기숙정기미(TBGE);연구료최화제류형、ECH여TBA물료비、최화제용량、가성반응온도급시간등인소대TBGE수솔적영향,용기상색보법분석료산품중TBGE함량,GC-MS화FT-IR등표정료산물결구。실험결과표명,삼불화붕(BF3)-을미시성능우량적최화제;재BF3-을미적용량위TBA질량적3.0%、가성반응적온도화시간분별위50.0℃화5.0 h、nECH/nTBA위2.5적조건하,TBGE적수솔가체85%이상;기상색보적분석결과표명산품중TBGE함량재99.0%이상。
The tert-butyl glycidyl ether(TBGE) was synthesized through additive reaction and cyclic action with epichlorohydrin(ECH) and tert-butanol(TBA) as raw materials.The effects of catalyst type,the amount of catalyst,the temperature and time of addition reaction and the molar ratio of ECH versus TBA on the yield of TBGE were investigated.The content of TBGE in product was determined by GC and the structure of product was characterized by GC-MS and FT-IR.When the BF3-etherate was utilized as catalyst and the mass ratio of BF3-etherate versus TBA was 3.0%,the temperature of addition reaction was 50.0 ℃,reaction time was 5.0 h,and the molar ratio of ECH versus TBA was 2.5,experimental results indicated the yield of TBGE was above 85 %.The result of GC showed the content of TBGE in the product surpassed 99.0%.