高校化学工程学报
高校化學工程學報
고교화학공정학보
JOURNAL OF CHEMICAL ENGINEERING OF CHINESE UNIVERSITIES
2015年
2期
305-311
,共7页
黄志钰%李英明%潘延波%李莎莎%杨伯伦
黃誌鈺%李英明%潘延波%李莎莎%楊伯倫
황지옥%리영명%반연파%리사사%양백륜
溶胶凝胶法%程序升温还原%磷化镍%加氢脱硫%制备放大
溶膠凝膠法%程序升溫還原%燐化鎳%加氫脫硫%製備放大
용효응효법%정서승온환원%린화얼%가경탈류%제비방대
sol-gel method%temperature-programmed reduction%nickel phosphide%hydrodesulfurization%preparation scale-up
按照单位体积搅拌功率恒等的放大准则,采用不同规格的反应釜以溶胶凝胶法(sol-gel)制备TiO 2-Al 2 O 3复合载体;依据还原气体线速度恒等的放大准则,在不同规格管式炉中以程序升温还原法(TPR)制备Ni 2 P/TiO 2-Al 2 O 3催化剂,并在连续固定床反应器中考察催化剂的加氢脱硫性能,以研究凝胶、TPR这两个催化剂制备关键过程的“放大效应”。结果表明,放大制备的载体物化性质与小试结果相当,放大制备的催化剂在温度603 K、压力2.5 MPa、质量空速2 h?1、氢油体积比500的条件下对含硫量为0.1%(wt)的二苯并噻吩(DBT)/环己烷溶液进行90 h的加氢脱硫反应,转化率达到99.4%,模型油品中硫含量降至6 ppm,其结果也与小试相同,表明上述载体以及催化剂制备工艺可靠、重复性好,有望实现规模化制备。
按照單位體積攪拌功率恆等的放大準則,採用不同規格的反應釜以溶膠凝膠法(sol-gel)製備TiO 2-Al 2 O 3複閤載體;依據還原氣體線速度恆等的放大準則,在不同規格管式爐中以程序升溫還原法(TPR)製備Ni 2 P/TiO 2-Al 2 O 3催化劑,併在連續固定床反應器中攷察催化劑的加氫脫硫性能,以研究凝膠、TPR這兩箇催化劑製備關鍵過程的“放大效應”。結果錶明,放大製備的載體物化性質與小試結果相噹,放大製備的催化劑在溫度603 K、壓力2.5 MPa、質量空速2 h?1、氫油體積比500的條件下對含硫量為0.1%(wt)的二苯併噻吩(DBT)/環己烷溶液進行90 h的加氫脫硫反應,轉化率達到99.4%,模型油品中硫含量降至6 ppm,其結果也與小試相同,錶明上述載體以及催化劑製備工藝可靠、重複性好,有望實現規模化製備。
안조단위체적교반공솔항등적방대준칙,채용불동규격적반응부이용효응효법(sol-gel)제비TiO 2-Al 2 O 3복합재체;의거환원기체선속도항등적방대준칙,재불동규격관식로중이정서승온환원법(TPR)제비Ni 2 P/TiO 2-Al 2 O 3최화제,병재련속고정상반응기중고찰최화제적가경탈류성능,이연구응효、TPR저량개최화제제비관건과정적“방대효응”。결과표명,방대제비적재체물화성질여소시결과상당,방대제비적최화제재온도603 K、압력2.5 MPa、질량공속2 h?1、경유체적비500적조건하대함류량위0.1%(wt)적이분병새분(DBT)/배기완용액진행90 h적가경탈류반응,전화솔체도99.4%,모형유품중류함량강지6 ppm,기결과야여소시상동,표명상술재체이급최화제제비공예가고、중복성호,유망실현규모화제비。
Reactors with different specifications were used to prepare TiO2-Al2O3 composite supports by a sol-gel method (sol-gel). The scale-up process was followed the criterion of identical stirring power per unit volume. Tube furnaces with different sizes were used to prepare Ni2P/TiO2-Al2O3 catalysts by a temperature-programmed reduction (TPR) method in accordance with the scale-up criterion of identical reducing gas flow rate. The hydrodesulfurization performance of the catalysts was examined using a continuous fixed-bed reactor to investigate the “scale-up effect” in gelation and TPR processes (two key processes in catalyst preparation). The results show that the physical properties of the supports prepared in large scale is close to that prepared in small scale. Hydrodesulfurization at 603K, 2.5MPa, WHSV 2 h?1 and hydrogen/oil volume ratio of 500 for 90 h shows that the catalysts prepared in large scale achieves a conversion rate of 99.4%. The sulfur content in the model oil was reduced to 6 ppm, which was the same as the lab-scale test results. These results show that the preparation processes of the support and the catalyst are reliable and repeatable, and the scale-up of the catalyst is possible.