纳米催化无机膜集成技术的研究与应用
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摘要
纳米催化剂是新一代高性能的催化剂,具有高的催化活性、高的催化选择性、
良好的催化稳定性,具有巨大的研究与应用价值,已受到科学界、企业界、各国
政府的高度重视。经过多年的研究与开发,纳米催化剂的制备技术已日趋完善并
逐步走向产业化。但是,关于纳米催化剂的工业化应用还是很少,特别是那种非
负载型的悬浮态纳米催化剂,其主要原因之一是纳米催化剂的分离回收问题还没
有很好的解决。高梯度磁分离与无机膜分离是两种较好的分离回收悬浮态纳米催
化剂的技术,前者要求纳米催化剂或其载体具有高度饱和磁化强度而限制了它的
应用,后者的应用领域更广。因而,采用无机膜分离技术分离回收纳米催化剂以
解决纳米催化剂工程化应用的瓶颈问题已成为当前关注的焦点之一。
无机膜催化反应器是将催化反应与无机膜分离过程相结合的一种反应分离
耦合技术,已受到普遍关注。目前的无机膜催化反应过程研究还主要集中在气相
体系,对液相体系的研究相对较少,尤其是对催化剂处于悬浮态的液相催化反应
的研究。而使用悬浮态的催化剂可大大增加反应速率,提高催化剂的使用效率,
而且这一类膜反应器也比较容易放大,所以研究催化剂处于悬浮态的液相无机催
化膜反应器具有广阔的前景。
为实现悬浮态纳米催化剂的工业化应用,我们对纳米催化与无机膜分离的耦
合过程进行研究,主要从三个层次上展开研究工作:在对硝基苯酚制备对氨基苯
酚的过程中研究纳米镍的催化性能;以上述催化过程为模型反应,对分置式的纳
米催化无机膜反应器进行理论分析;在此基础上,针对分置式膜反应器的不足,
进一步开发一体式纳米催化无机膜反应器,通过过程强化研究该膜反应器中的膜
过滤行为,为一体式纳米催化无机膜反应器的应用提供基础数据与理论依据。
首先,在对氨基苯酚的合成反应中比较了纳米镍与骨架镍的催化性能。实验
结果显示,在同样的实验条件下,纳米镍的催化活性、稳定性、选择性均优于骨
架镍。纳米镍的小粒径效应、表面结构以及不存在内孔等因素导致纳米镍具有高
的催化活性、稳定性与选择性。采用氮气吸附、粒径分析等技术,对使用前后的
催化剂的比表面积、孔容、粒径进行表征分析。结果表明,比表面积不是决定镍
催化活性的唯一因素;纳米镍在反应中的团聚会导致纳米镍的失活;骨架镍催化
剂中的一些微孔被反应物或产物所堵塞是引起骨架镍失活的原因之一。可见,在
对硝基苯酚催化加氢制备对氨基苯酚的过程中,使用纳米镍作为催化剂,可大大
提高催化剂的使用效率。在此基础上,研究了纳米镍催化合成对氨基苯酚的本征
动力学,为纳米催化合成对氨基苯酚的工业生产提供基础数据。研究结果表明:
当搅拌速度大于 300rpm 时,外扩散的影响已消除;在反应温度 80-110℃时,氢
I
南 京 工 业 大 学 博 士 学 位 论 文
压 0.8MPa-1.9MPa,对硝基苯酚的初始浓度 37.94-249.97g·L-1的实验条件下,该
反应对氢气为 1.3 级,对对硝基苯酚为零级,反应的活化能为 32.62 kJ·mol-1。
其次,从采用陶瓷膜错流过滤技术分离回收纳米镍催化剂的可行性出发,研
究操作参数对膜过滤性能的影响,考察膜过滤过程对催化剂的粒径、催化活性、
悬浮液中颗粒浓度的影响,并对膜的污染与清洗进行详细的分析。结果表明,使
用平均孔径为 50 纳米的 ZrO2陶瓷膜可以将纳米镍催化剂完全截留。操作压力在
0.25MPa 左右时比较适宜。在实验范围内,随着膜面流速的增大,膜通量先减小
后增大,这主要与纳米镍催化剂的粒径分布、易吸附等特性有关。膜通量随着颗
粒浓度的增加而降低,随着温度的升高而线性增加。离心泵错流膜过滤过程对纳
米镍催化剂的粒径以及催化活性都没有影响,这对纳米催化-膜分离耦合系统的
稳定性操作是非常有利的。增加膜面流速有利于抑制悬浮液中纳米镍催化剂浓度
的降低。采用扫描电镜对污染膜的截面及表面进行微观表征;采用能量发散 X
衍射技术对膜的化学成份进行分析;根据 Darcy 定律对膜过滤阻力进行分析。结
果表明,纳米镍催化剂吸附在膜的表面上及堵塞部分膜孔造成的膜污染是膜通量
下降的主要原因。采用物理清洗加化学清洗的组合方法可以较好地恢复膜通量且
清洗重复性好。
然后,采用数学分析手段探讨了无机膜反应器的构型、反应级数等因素对三
种多相分置式催化无机膜反应器(连续搅拌釜式-无机膜反应器(简称
CST-MR)、间隙搅拌釜式-无机膜反应器(简称 BST-MR)、连续管式-无机膜
反应器(简称 PF-MR))所需反应体积大小的影响,并以反应体积为目标函数,
对于特定的反应确定最佳的分置式催化无机膜反应器。分析结果表明,对于像纳
米镍催化合成对氨基苯酚的零级反应而言,选择 CST-MR 比较适宜。通过对
CST-MR 中物料停留时间分布的分析可知,实际 CST-MR 系统中的物料停留时间
分布密度可以直接按无外循环的、容积不包括循环系统的全混流反应器(CSTR)
的停留时间分布密度来计算。
最后,从一体式膜反应过程中膜过滤(简称一体式膜过滤)的特点出发,实
验研究一体式膜过滤的强化,开发新型的一体式膜反应器,弥补分置式膜反应器
的不足,并为一体式纳米催化无机膜反应器的应用提供基础数据与理论依据。主
要
Nano-sized catalysts have received considerable attention for their excellent
catalytic properties. Up to now, various methods have been developed to prepare
nano-sized catalysts, and furthermore, a lot of nano-sized catalysts have been
commercially produced. But the large scale applications of nano-sized catalysts have
been still few, especially for these unsupported suspended nano-sized catalysts. One
of the main reasons is due to the fact that the problem of recovery of nano-sized
catalysts from product mixture has not been well resolved. High-gradient magnetic
separation and inorganic membrane separation are two main methods for recovering
nano-sized catalysts and the latter is more practicable. Therefore, applying inorganic
membrane separation in nanocatalysis is important for implementing the industrial
applications of nano-sized catalysts.
In recent years, inorganic membrane reactors have been paid many attentions,
but the research has been focused on gas-phase applications. A limited number of
studies are concerned with the applications of inorganic membrane reactors to liquid
phase reactions, especially for liquid phase reactions with catalysts in suspension.
In order to implement commercial applications of nano-sized catalysts, the
research work was carried out on coupling of nanocatalysis and inorganic membranes
in this dissertation: examining the catalytic properties of nano-sized nickel for the
preparation of p-aminophenol; theoretical analyzing side-stream nanocatalytic
inorganic membrane reactor for the preparation of p-aminophenol over nano-sized
nickel; designing a novel submerged inorganic membrane reactor to overcome the
shortage of side-stream membrane reactor and to enhance the membrane flux by
process intensification. These works will provide fundamental knowledge for the
application of nanocatalytic inorganic membrane reactor.
Firstly, catalytic properties of nano-sized nickel were investigated in the catalytic
hydrogenation of p-nitrophenol to p-aminophenol in comparison with conventional
Raney nickel, which is the commercially used catalyst. Experimental results showed
that the catalytic activity, stability and selectivity of nano-sized nickel were superior
to those of Raney nickel under the same reaction conditions. Particle size, surface
structure and absence of micropores might be responsible for nano-sized nickel’s
excellent catalytic properties. Fresh nickel and used nickel samples were characterized
by particle size analyzer and nitrogen sorption. The results indicated that aggregation
IV
南 京 工 业 大 学 博 士 学 位 论 文
of nanoparticles might lead to the deactivation of nano-sized nickel and jam of
micropores could be the major reason for the deactivation of Raney nickel. In
conclusion, nano-sized nickel was an efficient catalyst for the catalytic hydrogenation
of p-nitrophenol to p-aminophenol. The intrinsic kinetics of preparation of
p-aminophenol from p-nitrophenol over nano-sized nickel catalyst was also studied
under exclusion from effects of external diffusion and internal diffusion. Experimental
results showed that external diffusing influence could be eliminated when the
agitation rate was over 300 rpm. Under the conditions that the reaction temperature,
the hydrogen pressure, the initial concentration of p-nitrophenol were 80-110 C, 0.8
o
MPa-1.9 MPa, 37.94-249.97 g·L-1 respectively, the reaction was zeroth order with
respect to p-nitrophenol and 1.3 order with respect to hydrogen, and the activation
energy of the reaction was 32.62 kJ·mol-1.
Secondly, the feasibility of using cross-flow ultrafiltration technology to separate
the nano-sized nickel catalyst from a liquid was investigated. At the same time, effects
of operating conditions on the filtration performance were discussed. Other filtration
behaviors, such as membrane fouling and cleaning, were also studied. Experimental
results showed that the nano-sized nickel catalyst could be completely rejected by a
ceramic membrane with a mean pore size of
良好的催化稳定性,具有巨大的研究与应用价值,已受到科学界、企业界、各国
政府的高度重视。经过多年的研究与开发,纳米催化剂的制备技术已日趋完善并
逐步走向产业化。但是,关于纳米催化剂的工业化应用还是很少,特别是那种非
负载型的悬浮态纳米催化剂,其主要原因之一是纳米催化剂的分离回收问题还没
有很好的解决。高梯度磁分离与无机膜分离是两种较好的分离回收悬浮态纳米催
化剂的技术,前者要求纳米催化剂或其载体具有高度饱和磁化强度而限制了它的
应用,后者的应用领域更广。因而,采用无机膜分离技术分离回收纳米催化剂以
解决纳米催化剂工程化应用的瓶颈问题已成为当前关注的焦点之一。
无机膜催化反应器是将催化反应与无机膜分离过程相结合的一种反应分离
耦合技术,已受到普遍关注。目前的无机膜催化反应过程研究还主要集中在气相
体系,对液相体系的研究相对较少,尤其是对催化剂处于悬浮态的液相催化反应
的研究。而使用悬浮态的催化剂可大大增加反应速率,提高催化剂的使用效率,
而且这一类膜反应器也比较容易放大,所以研究催化剂处于悬浮态的液相无机催
化膜反应器具有广阔的前景。
为实现悬浮态纳米催化剂的工业化应用,我们对纳米催化与无机膜分离的耦
合过程进行研究,主要从三个层次上展开研究工作:在对硝基苯酚制备对氨基苯
酚的过程中研究纳米镍的催化性能;以上述催化过程为模型反应,对分置式的纳
米催化无机膜反应器进行理论分析;在此基础上,针对分置式膜反应器的不足,
进一步开发一体式纳米催化无机膜反应器,通过过程强化研究该膜反应器中的膜
过滤行为,为一体式纳米催化无机膜反应器的应用提供基础数据与理论依据。
首先,在对氨基苯酚的合成反应中比较了纳米镍与骨架镍的催化性能。实验
结果显示,在同样的实验条件下,纳米镍的催化活性、稳定性、选择性均优于骨
架镍。纳米镍的小粒径效应、表面结构以及不存在内孔等因素导致纳米镍具有高
的催化活性、稳定性与选择性。采用氮气吸附、粒径分析等技术,对使用前后的
催化剂的比表面积、孔容、粒径进行表征分析。结果表明,比表面积不是决定镍
催化活性的唯一因素;纳米镍在反应中的团聚会导致纳米镍的失活;骨架镍催化
剂中的一些微孔被反应物或产物所堵塞是引起骨架镍失活的原因之一。可见,在
对硝基苯酚催化加氢制备对氨基苯酚的过程中,使用纳米镍作为催化剂,可大大
提高催化剂的使用效率。在此基础上,研究了纳米镍催化合成对氨基苯酚的本征
动力学,为纳米催化合成对氨基苯酚的工业生产提供基础数据。研究结果表明:
当搅拌速度大于 300rpm 时,外扩散的影响已消除;在反应温度 80-110℃时,氢
I
南 京 工 业 大 学 博 士 学 位 论 文
压 0.8MPa-1.9MPa,对硝基苯酚的初始浓度 37.94-249.97g·L-1的实验条件下,该
反应对氢气为 1.3 级,对对硝基苯酚为零级,反应的活化能为 32.62 kJ·mol-1。
其次,从采用陶瓷膜错流过滤技术分离回收纳米镍催化剂的可行性出发,研
究操作参数对膜过滤性能的影响,考察膜过滤过程对催化剂的粒径、催化活性、
悬浮液中颗粒浓度的影响,并对膜的污染与清洗进行详细的分析。结果表明,使
用平均孔径为 50 纳米的 ZrO2陶瓷膜可以将纳米镍催化剂完全截留。操作压力在
0.25MPa 左右时比较适宜。在实验范围内,随着膜面流速的增大,膜通量先减小
后增大,这主要与纳米镍催化剂的粒径分布、易吸附等特性有关。膜通量随着颗
粒浓度的增加而降低,随着温度的升高而线性增加。离心泵错流膜过滤过程对纳
米镍催化剂的粒径以及催化活性都没有影响,这对纳米催化-膜分离耦合系统的
稳定性操作是非常有利的。增加膜面流速有利于抑制悬浮液中纳米镍催化剂浓度
的降低。采用扫描电镜对污染膜的截面及表面进行微观表征;采用能量发散 X
衍射技术对膜的化学成份进行分析;根据 Darcy 定律对膜过滤阻力进行分析。结
果表明,纳米镍催化剂吸附在膜的表面上及堵塞部分膜孔造成的膜污染是膜通量
下降的主要原因。采用物理清洗加化学清洗的组合方法可以较好地恢复膜通量且
清洗重复性好。
然后,采用数学分析手段探讨了无机膜反应器的构型、反应级数等因素对三
种多相分置式催化无机膜反应器(连续搅拌釜式-无机膜反应器(简称
CST-MR)、间隙搅拌釜式-无机膜反应器(简称 BST-MR)、连续管式-无机膜
反应器(简称 PF-MR))所需反应体积大小的影响,并以反应体积为目标函数,
对于特定的反应确定最佳的分置式催化无机膜反应器。分析结果表明,对于像纳
米镍催化合成对氨基苯酚的零级反应而言,选择 CST-MR 比较适宜。通过对
CST-MR 中物料停留时间分布的分析可知,实际 CST-MR 系统中的物料停留时间
分布密度可以直接按无外循环的、容积不包括循环系统的全混流反应器(CSTR)
的停留时间分布密度来计算。
最后,从一体式膜反应过程中膜过滤(简称一体式膜过滤)的特点出发,实
验研究一体式膜过滤的强化,开发新型的一体式膜反应器,弥补分置式膜反应器
的不足,并为一体式纳米催化无机膜反应器的应用提供基础数据与理论依据。主
要
Nano-sized catalysts have received considerable attention for their excellent
catalytic properties. Up to now, various methods have been developed to prepare
nano-sized catalysts, and furthermore, a lot of nano-sized catalysts have been
commercially produced. But the large scale applications of nano-sized catalysts have
been still few, especially for these unsupported suspended nano-sized catalysts. One
of the main reasons is due to the fact that the problem of recovery of nano-sized
catalysts from product mixture has not been well resolved. High-gradient magnetic
separation and inorganic membrane separation are two main methods for recovering
nano-sized catalysts and the latter is more practicable. Therefore, applying inorganic
membrane separation in nanocatalysis is important for implementing the industrial
applications of nano-sized catalysts.
In recent years, inorganic membrane reactors have been paid many attentions,
but the research has been focused on gas-phase applications. A limited number of
studies are concerned with the applications of inorganic membrane reactors to liquid
phase reactions, especially for liquid phase reactions with catalysts in suspension.
In order to implement commercial applications of nano-sized catalysts, the
research work was carried out on coupling of nanocatalysis and inorganic membranes
in this dissertation: examining the catalytic properties of nano-sized nickel for the
preparation of p-aminophenol; theoretical analyzing side-stream nanocatalytic
inorganic membrane reactor for the preparation of p-aminophenol over nano-sized
nickel; designing a novel submerged inorganic membrane reactor to overcome the
shortage of side-stream membrane reactor and to enhance the membrane flux by
process intensification. These works will provide fundamental knowledge for the
application of nanocatalytic inorganic membrane reactor.
Firstly, catalytic properties of nano-sized nickel were investigated in the catalytic
hydrogenation of p-nitrophenol to p-aminophenol in comparison with conventional
Raney nickel, which is the commercially used catalyst. Experimental results showed
that the catalytic activity, stability and selectivity of nano-sized nickel were superior
to those of Raney nickel under the same reaction conditions. Particle size, surface
structure and absence of micropores might be responsible for nano-sized nickel’s
excellent catalytic properties. Fresh nickel and used nickel samples were characterized
by particle size analyzer and nitrogen sorption. The results indicated that aggregation
IV
南 京 工 业 大 学 博 士 学 位 论 文
of nanoparticles might lead to the deactivation of nano-sized nickel and jam of
micropores could be the major reason for the deactivation of Raney nickel. In
conclusion, nano-sized nickel was an efficient catalyst for the catalytic hydrogenation
of p-nitrophenol to p-aminophenol. The intrinsic kinetics of preparation of
p-aminophenol from p-nitrophenol over nano-sized nickel catalyst was also studied
under exclusion from effects of external diffusion and internal diffusion. Experimental
results showed that external diffusing influence could be eliminated when the
agitation rate was over 300 rpm. Under the conditions that the reaction temperature,
the hydrogen pressure, the initial concentration of p-nitrophenol were 80-110 C, 0.8
o
MPa-1.9 MPa, 37.94-249.97 g·L-1 respectively, the reaction was zeroth order with
respect to p-nitrophenol and 1.3 order with respect to hydrogen, and the activation
energy of the reaction was 32.62 kJ·mol-1.
Secondly, the feasibility of using cross-flow ultrafiltration technology to separate
the nano-sized nickel catalyst from a liquid was investigated. At the same time, effects
of operating conditions on the filtration performance were discussed. Other filtration
behaviors, such as membrane fouling and cleaning, were also studied. Experimental
results showed that the nano-sized nickel catalyst could be completely rejected by a
ceramic membrane with a mean pore size of
引文
[1] 胡迁林 我国催化技术及催化剂的发展现状,当代化工,2001,30:2-6.
[2] 张立德 纳米材料技术的发展趋势和应用机遇,世界科技研究与发展,2002,24:18-22.
[3] 张立德 纳米材料和技术的战略地位、发展趋势和应用,中国高新技术企业,2000:
4-6.
[4] 周忠清,金国山 金超微粒子催化剂的新进展,现代化工,1999,19:19-21.
[5] 张玉军,陈杰瑢 油脂加氢催化剂研究现状及发展趋势,工业催化,2002,10:23-26.
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