化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2014年
10期
2655-2660
,共6页
2-乙酰噻吩%连续反应%分子筛%失活%催化
2-乙酰噻吩%連續反應%分子篩%失活%催化
2-을선새분%련속반응%분자사%실활%최화
2-acetyl thiophene%continuous reaction%molecular sieves%deactivation%catalyst
在滴流床反应器中，以C25沸石分子筛为催化剂，噻吩和乙酸酐为原料对噻吩酰化合成2-乙酰噻吩进行了连续反应实验研究。通过正交试验研究了反应温度、原料配比、进料流量对噻吩 Friedel-Crafts 酰基化反应的影响，确定了最佳反应条件：反应温度70℃，噻吩与乙酸酐摩尔配比1∶2，进料流量0.05mL/min。考察了副产物乙酸对反应的影响，确定了噻吩、乙酸酐和乙酸的最佳摩尔比为1∶2∶1，在最佳反应条件下，单位质量催化剂的2-乙酰噻吩产量为15.10g，催化剂寿命是4215min，噻吩初始转化率高达99.98%。采用固体13C、27Al 核磁共振技术、热重分析对催化剂进行表征，结果表明，催化剂主要催化活性在 B 酸位，失活类型为高沸点物质的积炭失活。
在滴流床反應器中，以C25沸石分子篩為催化劑，噻吩和乙痠酐為原料對噻吩酰化閤成2-乙酰噻吩進行瞭連續反應實驗研究。通過正交試驗研究瞭反應溫度、原料配比、進料流量對噻吩 Friedel-Crafts 酰基化反應的影響，確定瞭最佳反應條件：反應溫度70℃，噻吩與乙痠酐摩爾配比1∶2，進料流量0.05mL/min。攷察瞭副產物乙痠對反應的影響，確定瞭噻吩、乙痠酐和乙痠的最佳摩爾比為1∶2∶1，在最佳反應條件下，單位質量催化劑的2-乙酰噻吩產量為15.10g，催化劑壽命是4215min，噻吩初始轉化率高達99.98%。採用固體13C、27Al 覈磁共振技術、熱重分析對催化劑進行錶徵，結果錶明，催化劑主要催化活性在 B 痠位，失活類型為高沸點物質的積炭失活。
재적류상반응기중，이C25비석분자사위최화제，새분화을산항위원료대새분선화합성2-을선새분진행료련속반응실험연구。통과정교시험연구료반응온도、원료배비、진료류량대새분 Friedel-Crafts 선기화반응적영향，학정료최가반응조건：반응온도70℃，새분여을산항마이배비1∶2，진료류량0.05mL/min。고찰료부산물을산대반응적영향，학정료새분、을산항화을산적최가마이비위1∶2∶1，재최가반응조건하，단위질량최화제적2-을선새분산량위15.10g，최화제수명시4215min，새분초시전화솔고체99.98%。채용고체13C、27Al 핵자공진기술、열중분석대최화제진행표정，결과표명，최화제주요최화활성재 B 산위，실활류형위고비점물질적적탄실활。
With C25 zeolite molecular sieve as catalyst,thiophene and acetic anhydride as raw materials,continuous synthesis of 2-acetyl thiophene was conducted in a trickle bed reactor. The effects of reaction temperature,molar ratio of raw materials,feed flow rate on the Friedel-Crafts acylation reaction were investigated via orthogonal experiment. The optimum reaction condition was:reaction temperature 70℃,molar ratio of thiophene and acetic anhydride 1∶2,feed flow rate 0.05mL/min. Considering the influence of acetic acid on the reaction,the best molar ratio of thiophene,acetic anhydride and acetic acid was 1∶2∶1. Under those conditions,output of 2-acetyl thiophene was 15.10g per unit mass of catalyst,catalyst service life was 4215 min and initial conversion of thiophene could reach 99.98%. The catalyst was characterized with 13C NMR MAS,27Al NMR MAS,and TGA analysis. Bronsted acid sites played an important role in catalysis and the main deactivation type was coking deactivation by compounds with high boiling point.
