石油化工
石油化工
석유화공
PETROCHEMICAL TECHNOLOGY
2009年
12期
1281-1285
,共5页
黄绍祥%黎先财%黄晓文%徐庆荣%杨沂凤%刘厚凡
黃紹祥%黎先財%黃曉文%徐慶榮%楊沂鳳%劉厚凡
황소상%려선재%황효문%서경영%양기봉%류후범
介孔SBA-15分子筛%三氧化钨催化剂%噻吩%氧化萃取脱硫%1-甲基-2-吡咯烷酮
介孔SBA-15分子篩%三氧化鎢催化劑%噻吩%氧化萃取脫硫%1-甲基-2-吡咯烷酮
개공SBA-15분자사%삼양화오최화제%새분%양화췌취탈류%1-갑기-2-필각완동
mesoporous SBA-15 molecular sieve%tungsten trioxide catalyst%thiophene%oxidative-extraction desulfurization%1-methyl-2-pyrrolidone
以介孔SBA-15分子筛为载体,采用两种不同钨源(H_2WO_4和H_2C_2O_4、H_2WO_4和H_2O_2)通过浸渍法制备了WO_3/SBA-15催化剂;采用X射线衍射和傅里叶变换红外光谱法对介孔SBA-15分子筛和WO_3/SBA-15催化剂进行了表征;以硫含量为500 μg/g的模拟汽油为原料进行氧化脱硫反应,反应后油相用1-甲基-2-吡咯烷酮萃取,考察了萃取剂用量、催化剂用量、氧化反应温度和反应时间对脱硫率的影响.表征结果显示,WO_3/SBA-15催化剂有规则的二维六方介孔结构,WO_3在载体上高度分散.实验结果表明,以H_2WO_4和H_2C_2O_4为钨源制备的WO_3/SBA-15催化剂的脱硫效果较好,在反应温度320 K、反应时间120 min、模拟汽油60 mL、催化剂用量0.12 g、双氧水0.57 mL、萃取剂与模拟汽油体积比0.50、萃取时间5 min的条件下,脱硫率可达94.05%.
以介孔SBA-15分子篩為載體,採用兩種不同鎢源(H_2WO_4和H_2C_2O_4、H_2WO_4和H_2O_2)通過浸漬法製備瞭WO_3/SBA-15催化劑;採用X射線衍射和傅裏葉變換紅外光譜法對介孔SBA-15分子篩和WO_3/SBA-15催化劑進行瞭錶徵;以硫含量為500 μg/g的模擬汽油為原料進行氧化脫硫反應,反應後油相用1-甲基-2-吡咯烷酮萃取,攷察瞭萃取劑用量、催化劑用量、氧化反應溫度和反應時間對脫硫率的影響.錶徵結果顯示,WO_3/SBA-15催化劑有規則的二維六方介孔結構,WO_3在載體上高度分散.實驗結果錶明,以H_2WO_4和H_2C_2O_4為鎢源製備的WO_3/SBA-15催化劑的脫硫效果較好,在反應溫度320 K、反應時間120 min、模擬汽油60 mL、催化劑用量0.12 g、雙氧水0.57 mL、萃取劑與模擬汽油體積比0.50、萃取時間5 min的條件下,脫硫率可達94.05%.
이개공SBA-15분자사위재체,채용량충불동오원(H_2WO_4화H_2C_2O_4、H_2WO_4화H_2O_2)통과침지법제비료WO_3/SBA-15최화제;채용X사선연사화부리협변환홍외광보법대개공SBA-15분자사화WO_3/SBA-15최화제진행료표정;이류함량위500 μg/g적모의기유위원료진행양화탈류반응,반응후유상용1-갑기-2-필각완동췌취,고찰료췌취제용량、최화제용량、양화반응온도화반응시간대탈류솔적영향.표정결과현시,WO_3/SBA-15최화제유규칙적이유륙방개공결구,WO_3재재체상고도분산.실험결과표명,이H_2WO_4화H_2C_2O_4위오원제비적WO_3/SBA-15최화제적탈류효과교호,재반응온도320 K、반응시간120 min、모의기유60 mL、최화제용량0.12 g、쌍양수0.57 mL、췌취제여모의기유체적비0.50、췌취시간5 min적조건하,탈류솔가체94.05%.
WO_3/SBA-15 catalysts were prepared by impregnation from two alternative tungsten sources(tungstic acid, oxalic acid and tungstic acid, hydrogen peroxide) with mesoporous SBA-15 molecular sieves as support. The catalysts were characterized by means of XRD and FTIR. Oxidative desulfurization of model gasoline(sulfur content 500 μg/g) was catalyzed by the two WO_3/SBA-15 catalysts separately and the oil phase was extracted by 1-methyl-2-pyrrolidone after reaction. Effects of extractant dosage, catalyst amount, reaction temperature and time on the desulfurization rate were investigated. WO_3/SBA-15 catalysts still kept ordered two-dimensional hexagonal mesoporous structure of the support, and WO3 species was highly dispersed on it. The catalyst prepared from tungstic acid and oxalic acid showed higher activity in oxidative desulfurization than the counterpart. The optimized oxidative desulfurization conditions were: reaction temperature 320 K, reaction time 120 min, model gasoline 60 mL,catalyst dosage 0.12 g and 30%(w)H_2O_2 solution 0.57 mL. After seperation of catalyst,desulfurization rate of gasoline was determined by extraction with 1-methyl-2-pyrrolidone as extractant, volume ratio of extractant to model gasoline 0.50, extraction time 5 min, the desulfurization rate was 94.05%.