CN1107704C - 裂解汽油选择性加氢催化剂 - Google Patents

裂解汽油选择性加氢催化剂 Download PDF

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CN1107704C
CN1107704C CN00101797A CN00101797A CN1107704C CN 1107704 C CN1107704 C CN 1107704C CN 00101797 A CN00101797 A CN 00101797A CN 00101797 A CN00101797 A CN 00101797A CN 1107704 C CN1107704 C CN 1107704C
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catalyst
pore volume
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pyrolysis gasoline
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李斯琴
门晓棠
刘根生
梁顺琴
张小工
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Lanzhou Petrochemical Institute Of China Petrochemical Corp
Petrochina Lanzhou Petrochemical Co
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/32—Selective hydrogenation of the diolefin or acetylene compounds
    • C10G45/34—Selective hydrogenation of the diolefin or acetylene compounds characterised by the catalyst used
    • C10G45/40—Selective hydrogenation of the diolefin or acetylene compounds characterised by the catalyst used containing platinum group metals or compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/58—Platinum group metals with alkali- or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/613—10-100 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/615—100-500 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/63—Pore volume
    • B01J35/635—0.5-1.0 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/64—Pore diameter
    • B01J35/647—2-50 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/66—Pore distribution
    • B01J35/67—Pore distribution monomodal

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

本发明涉及一种裂解汽油选择性加氢催化剂，载体为δ、α混合型氧化铝，比孔容为0.5～0.9ml/g，其中40～200的孔容占总孔容积的85%以上，孔径分布集中，比表面为70～140m2/g，氧化铝载体中α晶型占0.1～5%，活性组份除含贵金属钯以外，还可含其它元素。本发明的催化剂在处理物料量大(以新鲜油计空速可达4.0～6.0h-1)，杂质含量高的原料时，长期运转化学稳定性和热稳定性好，容胶性能好，积炭量低，寿命长，且制备工艺简单。

Description

裂解汽油选择性加氢催化剂
本发明涉及一种裂解汽油选择性加氢催化剂。
目前工业化裂解汽油选择性加氢催化剂仍以钯基催化剂为主，也有加有助剂的钯催化剂，助活性组份多为IA族元素。对于杂质较高的裂解汽油原料，仍有沿袭非贵金属镍系催化剂的。钯基催化剂由于具有启动温度低，加氢活性高，处理物料量大，催化剂寿命长等优点而明显优于镍系催化剂，如US4410455、ZL91109503.9等。但是当裂解汽油中双烯含量高，并含有砷、胶质等杂质时，已工业化钯基催化剂有很多难以在设计空速下稳定或长周期运行，经常是催化剂的设计空速虽能达到4.7h-1(新鲜进料)，实际运行时由于原料过重，杂质过多而只能降空速为2.8h-1操作。
本发明的目的在于提供一种适宜处理高杂质含量物料和适宜在高空速下进行操作的钯系加氢催化剂。
本发明所述的催化剂是由δ、α混合型氧化铝负载贵金属钯及碱金属或碱土金属化合物构成，活性组份在载体表面呈蛋壳型分布，以δ、α混合型氧化铝载体为基准，钯的含量为0.05～0.4％，碱金属和/或碱土金属的加入量为0.05～2.0％，催化剂载体比孔容为0.5～0.9ml/g，其中40～200的孔容占总孔容积的85％以上，最好100～200的孔容达总孔容积的65％～80％，孔径分布集中，比表面为70～140m2/g，氧化铝载体中α晶型占0.1～5％，其形状可以是机械打片型，也可以是三叶草或圆柱挤条，载体颗粒形状不影响本发明的实施。
本发明的催化剂除使用上述具有一定孔结构的δ、α混合型氧化铝，负载贵金属钯及碱金属或碱土金属化合物外还可加入助活性组份，助活性组份选自元素周期表的第VIB或IB族元素中的一种，助活性组份与Pd重量比为0.2～2∶1。
本发明催化剂的制备方法与普通壳层催化剂浸渍技术相同：先用一种能与浸渍液互溶的液体(如脱离子水)预浸载体，再用含有活性组份的盐溶液浸渍经预浸的δ、α混合型氧化铝载体，浸渍后的载体经洗涤、干燥，在空气中焙烧即得氧化型催化剂成品。成品催化剂只需在反应器中通氢气还原即可使用。
本发明中助活性组份可与Pd形成络合物，有利于Pd颗粒的均匀分布，提高Pd的利用率，减少Pd的流失，延长催化剂寿命；碱金属能改变载体表面的酸碱性，有利于降低加氢过程中胶质、炭质的沉积，孔分布集中，有减小内扩散阻力的作用；而较大的比孔容对处理物料量大，杂质含量高的物料是有利的，综合上述各种因素，使本发明的催化剂特别适宜处理高杂质含量物料和适宜在高空速下进行加氢。如处理胶质≤60mg/100ml，双烯值≤40克碘/100克油的全馏份裂解汽油，尤其可在空速4.0～6.0h-1(新鲜油)的条件下对C6～C8中间馏份油的加氢。
本发明的催化剂优点在于：处理物料量大(C6～C8中间馏份油，以新鲜油计空速可达4.0～6.0h-1)，杂质含量高的原料时，加氢活性高，选择性好，长期运转化学稳定性和热稳定性好，容胶性能好，积炭量低，寿命长，且制备工艺简单。
下面通过实施例具体说明本发明。
实施例1、2、3、4、5、6：
催化剂的制备采用经典的浸渍制备壳层型催化剂方法，即以脱离子水预浸载体，然后滤干水份，用含有活性组份的溶液浸渍载体，浸渍后的载体经洗涤、干燥，在空气中焙烧即可制得本发明的壳层型双金属钯催化剂，催化剂的外观为淡褐色，三叶草挤条，规格为φ2.8～3.2×3～10mm，催化剂的物性如表1所示。
比较例：
采用ZL911095303.9的方法制备得到的单金属钯催化剂，催化剂的外观为淡褐色，圆柱型打片成形，规格为φ4×4mm，催化剂的物性如表1所示。
                  表1实施例、比较例中得到的催化剂物性
         项目                           实施例  比较例
   1    2   3   4    5    6
载体   比表面m2/g    81    95   102   110    125    109   102
  比孔容ml/g    0.62    0.65   0.73   0.73    0.78    0.69   0.51
  孔分布：％40～200 88 86 95 91 90 89 72
  100～200    72    69   75   70    67    71   9
  α晶型所占比例％    0.8    0.7   1.0   1.9    2.5    1.3   6.0
  堆密度g/ml    0.57    0.59   0.60   0.64    0.58    0.61   0.79
催化剂   钯含量wt％    0.30    0.40   0.25   0.30    0.28    0.28   0.30
  助活性组份含量wt％    Cu0.03    Ag0.025   Mo1.0   Cu1.4    Cr2.0    --   --
  碱金属含量wt％    --    Na0.17   K0.47   Li0.92    --    Li0.92   --
碱土金属含量wt％ Mg0.06 -- Ba0.14 -- Ca1.56 -- --
将实施例1、2、3、4、5、6与比较例的催化剂在300ml绝热床上进行1000小时活性评价，评价结果见表2。
          表2实施例、比较例中得到的催化剂加氢性能※
           项目                                  实施例    比较例
    1     2     3     4    5     6
操作条件 温度℃     45     45     45     45    45     45     50
新鲜油空速h-1     5.0     4.5     5.5     5.5    6.0     5.0     4.0
压力MPa     2.8     2.8     2.8     2.8    2.8     2.8     2.8
氢油比v/v     50∶1     50∶1     50∶1     50∶1    50∶1     50∶1     50∶1
加氢后产品双烯值*克碘/100克油 200小时     0.82     0.79     0.44     0.58    0.73     1.06     2.23
500小时     0.94     0.98     0.91     0.97    1.06     1.77     2.65
750小时     1.06     1.02     1.02     1.08    1.29     1.98     2.94
1000小时     1.32     1.08     1.18     1.22    1.68     2.05     3.02
          容胶量％     7.8     6.9     6.5     7.0    8.7     6.7     10.6
※：评价中所用原料油双烯值为30～40克碘/100克油，胶质≤60mg/100ml；750小时前所用原料油为裂解汽油C6～C8中间馏份，750～1000小时切换成裂解汽油全馏份原料油。
*：油品中双烯值的测定方法为苹果酸酐法。
表3是实施例4与比较例的催化剂在300m1绝热床上于高空速条件下加氢性能的对比评价结果，评价中所用原料为裂解汽油C6～C8中间馏份，双烯值为30～40克碘/100克油，胶质小于60mg/100ml。
表3实施例4、比较例中得到的催化剂在高空速条件下加氢性能对比
          项目   实施例4     比较例
操作条件  温度℃     50     50
 压力MPa     2.8     2.8
 氢油比v/v     50∶1     50∶1
 新鲜油空速h-1     6.0     6.0
 循环比     3∶1     3∶1
 总空速h-1     24     24
  加氢后产品双烯值克碘/100克油  150小时     0.61     3.28
 300小时     0.88     5.79
 500小时     1.05     6.32
            容胶量％     6.4     9.3

Claims (4)

1.一种裂解汽油选择性加氢催化剂，其特征在于催化剂是由δ、α混合型氧化铝负载贵金属钯，活性组份在载体表面呈蛋壳型分布，以δ、α混合型氧化铝载体为基准，钯的含量为0.05～0.4wt％，碱金属和/或碱土金属的加入量为0.05～2.0wt％，催化剂载体比孔容为0.5～0.9ml/g，其中40～200的孔占总孔容积的85％以上，比表面为70～140m2/g，氧化铝载体中α晶型占0.1～5％。
2.根据权利要求1所述的加氢催化剂，其特征在于催化剂载体100～200的孔容达总孔容积的65％～80％。
3.根据权利要求1所述的加氢催化剂，其特征在于催化剂除负载有贵金属钯外，还负载有助活性组份，助活性组份选自元素周期表的第VIB或IB族元素中的一种，助活性组份与Pd重量比为0.2～2∶1。
4.根据权利要求1或2或3所述的加氢催化剂，其特征在于该催化剂适用于裂解汽油全馏份和C6～C8中间馏份油的加氢。
CN00101797A 2000-02-03 2000-02-03 裂解汽油选择性加氢催化剂 Expired - Fee Related CN1107704C (zh)

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CN1317364C (zh) * 2003-12-31 2007-05-23 中国石油化工股份有限公司北京燕山分公司研究院 用于裂解汽油重馏分选择加氢的催化剂、其制备方法及其应用
CN101121899B (zh) * 2006-08-11 2010-05-12 中国石油化工股份有限公司 用于全馏分裂解汽油选择性加氢的方法
CN101191079B (zh) * 2006-11-21 2011-03-23 中国石油化工股份有限公司上海石油化工研究院 用于全馏分裂解汽油选择性加氢的方法
CN101423775B (zh) 2007-11-01 2010-05-12 中国石油天然气股份有限公司 一种选择性镍系加氢催化剂及其制备方法
CN101433841B (zh) * 2007-12-13 2010-04-14 中国石油天然气股份有限公司 一种选择性加氢催化剂及其制备方法
CN101890351B (zh) * 2009-05-21 2012-10-24 中国石油化工股份有限公司 蛋壳型镍基催化剂
CN102744066A (zh) * 2012-05-08 2012-10-24 中国石油化工股份有限公司 一种流化床用硝基苯加氢制苯胺催化剂
CN103666548B (zh) * 2012-09-04 2015-12-02 中国石油天然气股份有限公司 一种汽油的选择性加氢方法
CN104415797B (zh) * 2013-08-27 2016-08-17 中国石油化工股份有限公司 一种裂解汽油选择加氢催化剂及其制备方法和应用
CN104645981B (zh) * 2013-11-19 2017-02-15 中国石油天然气股份有限公司 一种裂解汽油加氢催化剂及其制备方法
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