CN1143668A - 重质石油和蒸馏残余物转化成馏出液的方法 - Google Patents
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Abstract
用于转化重质石油或蒸馏残余物成蒸馏液的方法包括下述步骤：使重质石油或蒸馏残余物与一种适当的氢化催化剂混合并将所得的混合物送入加氢处理反应器中，引入氢气或氢气和H2S的混合物；将含有加氢处理反应产物和淤浆中的催化剂的物流送入蒸馏区，在该区分离出大多数挥发馏分；将蒸馏步骤中获得的高沸点馏分送入脱沥青步骤，得到两股物流，一股由脱沥青油(DAO)组成，另一股由沥青质、淤浆中的催化剂、可能有的焦炭和来自原料的富集的金属组成。
Description
本发明涉及一种利用淤浆中的氢化催化剂转化重质石油和蒸馏残余物的方法，所述催化剂被回收并循环而无需再生。
重质石油和石油脚的转化可主要按两种方式进行：一种是仅用加热方式，另一种是加氢处理方式。
目前的研究主要针对加氢处理进行的，这是由于热处理有涉及副产物特别是焦炭(获得量甚至高于原料的30％(wt))的处理和转化产品质量差的问题。
加氢化程由在氢气和适当的催化剂存在下处理原料组成。
目前市场上的加氢转化技术使用固定床或流化床反应器和一般由载于二氧化硅/氧化铝(或等同物)上的一种或多种过渡金属(Mo、W、Ni、Co等)组成的催化剂。
固定床技术在处理含有高百分比杂原子、金属和沥青质的特别重质原料时有相当大的问题，例如这些杂质引起催化剂的迅速失活。
为处理这些原料，已开发并出售了流化床技术，这种技术有令人感兴趣的性能但非常复杂且成本高。
用淤浆中的催化剂操作的加氢处理技术可能是一种克服固定床或流化床技术的缺点的有吸引力的方案。事实上淤浆法具有原料的广泛适应性和以转化率和提高等级表示的高的性能的综合优点，而且从技术方面来说是“简单的”。
淤浆技术特征是存在平均粒径非常小的并有效地分散在介质中的催化剂颗粒；由于该原因，加氢过程在反应器的所有位置更容易且更直接地进行。焦炭的生成大大减少并且原料的升级高。
催化剂可以作为具有足够小的粒径(US4303634)的粉末或者作为油溶性前体(US5288681)加入。在后面这种情况下，催化剂(一般是金属硫化物)的活化态通过所用的化合物的热分解在其反应过程中或在适当的预处理之后“就地”生成(US4470295)。
分散的催化剂的金属成分一般是一种或多种过渡金属(优选Mo、Ni或Co)。
使用分散的催化剂，虽然解决了上述技术的大部分问题，但仍有主要涉及催化剂自身的寿命周期的缺点。
使用这些催化剂的方法(前体种类、浓度等)在实际中很重要，关系到成本和对环境的影响。
催化剂可以在低浓度(几百ppm)下使用有“一次性”的优点，但这种情况下反应产物的升级不够。如果在较高的催化剂浓度(数千ppm的金属)下操作，需要回收催化剂。
离开反应器的催化剂可以通过用常规方法如滗析、离心或过滤法(US3240718；US4762812)由加氢处理获得的(优选从反应器下游的蒸馏塔底部获得的)产物分离来回收。部分催化剂可以不用进一步处理就循环到加氢过程中。然而，用公知的加氢处理法回收的催化剂一般有比新鲜催化剂低的活性，并且需要适当的再生步骤来恢复催化活性并使至少一部分催化剂循环到加氢处理反应器中。
我们意外地发现一种新方法，该方法能够使回收的催化剂循环到加氢处理反应器中无需进一步再生处理，同时获得质量好的产品而不产生残余物(“零精制残余”)。
本发明的重质石油或蒸馏残余物转化成馏出液的方法包括下列步骤：——使重质石油或蒸馏残余物与一种适当的加氢催化剂混合，并将所得到的混合物送入一个加氢处理反应器中，引入氢气或氢气和H2S的混合物；——将含加氢处理反应产物和淤浆中的催化剂的物流送入蒸馏区，在该区分离出大部分挥发性馏分；——将蒸馏步骤中获得的高沸点馏分送入脱沥青步骤，得到两股物流，一股由脱沥青油(DAO)组成，另一股由沥青质、淤浆中的催化剂、可能有的焦炭和来自初始进料的富集的金属组成；——使至少60％、优选至少80％的由沥青质、淤浆中的催化剂、视需要存在的焦炭和富集的金属组成的物流循环到加氢处理区中。
所用的催化剂可选自可由易分解的油溶性前体(环烷酸金属盐、磷酸的金属衍生物、羰基金属等)得到的那些或者基于一种或多种过渡金属如Ni、Co和Mo的预先形成的化合物：由于其高的催化活性，后者是优选的。
加氢处理步骤优选在370-480℃之间的温度，更优选在380-420℃之间的温度，和在30-300大气压之间的压力，更优选在100-180大气压之间的压力下进行。
脱沥青步骤优选通过一种溶剂(例如有3-6个碳原子的石蜡)萃取法一般在40-200℃之间的温度和1-50大气压之间的压力下进行。
蒸馏步骤可以借助于一个或多个塔在大气压和/或真空下进行。
现在借助于附图描述本发明的优选实施方案，然而它并不限制本发明的范围。
重质石油或蒸馏残余物(1)与新鲜催化剂(2)混合并进入氢化反应器(H)中，将氢气(或氢气/H2S混合物)(3)加入该反应器中。物流(4)离开反应器，含有反应产物和淤浆中的催化剂，在一蒸馏塔(D)中将其分馏，轻馏分(D1、D2、D3、Dn)与蒸馏残余物(5)分开。
该残余物(5)被送入脱沥青单元(E)，用一种溶剂进行萃取操作。从脱沥青单元(E)得到两股物流：一股(6)由脱沥青油(DAO)组成，另一股(7)由沥青质、焦炭和淤浆中催化剂组成。
物流(7)除了进行冲洗(9)以外的全部或大部分(8)进行循环，在与适量的新鲜原料(1)和任选的新鲜催化剂(2)混合后进入加氢处理反应器(H)。
下面的实例有助于更好地理解本发明，但并不以任何方式限制本发明。实例按图1中表示的流程图进行下面的实验：
加氢处理步骤：反应器：30CC，钢质结构，设有毛细搅拌原料：沥青质含量等于21.6％(wt)的Belayim原油真空残余物10g前体：环烷酸钼盐3000ppm的Mo/原料温度：400℃压力：170大气压的氢气停留时间：4小时脱沥青步骤脱沥青剂∶正戊烷400CC温度：室温压力：大气压三次循环后的出口处物流：——脱沥青油(DAO)：相对原料的50％(wt)——物流(7)由下述物质组成：—沥青质：相对原料的22％(wt)—焦炭：相对原料的5％(wt)—分散的催化剂：其100％进入反应器循环：
100％的物流(7)与这样的量的真空残余物混合使得总能得到相同的初始量的原料(10g)。
气体和轻馏分在脱沥青之前用常规的实验室方法分离。
比较在3次循环后回收的和1次循环后回收的DAO的某些特性数据(％S，Ni、V的ppm)，可以看到该量没有显著变化，从而看来并不存在催化剂的特别的失活问题(见表I)。
图2表示与沥青质的反应速度有关的结果，借助于条线图来表示，该图横坐标是循环次数且纵坐标是C5沥青质的百分比(其中C为焦炭；ar为回收的沥青质；at为沥青质的理论积累；ac为沥青质＋焦炭)。
有关沥青质的理论积累的数据是通过假设“新鲜的”沥青质约50％的转化率(正如用新鲜原料的第一次试验过程中出现的)和回收的那些的零转化率而计算出的。
将这些数据与实验获得的那些进行比较，可注意到回收的沥青质成分还在后续处理过程中进一步转化。
该图表还表明焦炭的百分比，所述焦炭是在步骤(I)过程中产生的并与沥青质一起循环。
表1
％S ppmNi/V ％CCRDAO第1次循环后 2.2 ＜5 7.4DAO第2次循环后 2.2 ＜5 7.3DAO第3次循环后 2.4 ＜5 6.6
Claims (9)
1.利用淤浆中的氢化催化剂转化重质石油和蒸馏残余物成为馏出液的方法，其特征是包括下述步骤：——使重质石油或蒸馏残余物与一种适当的氢化催化剂混合并将所得的混合物送入加氢处理反应器中，引入氢气或氢气和H2S的混合物；——将含有加氢处理反应产物和淤浆中的催化剂的物流送入蒸馏区，大多数挥发性馏分在该区被分开；——将蒸馏步骤中获得的高沸点馏分送入脱沥青步骤，得到两股物流，一股由脱沥青油(DAO)组成，另一股由沥青质、淤浆中催化剂、可能有的焦炭和来自原料的富集的金属组成；——使至少60％的由沥青质、淤浆中的催化剂、视需要存在的焦炭和富集的金属组成的物流循环到加氢处理区中。
2.按权利要求1的方法，其中至少80％的由沥青质、淤浆中的催化剂和可能有的焦炭组成的物流循环到加氢处理区。
3.按权利要求1或2的方法，其中加氢处理步骤在370和480℃之间的温度和在30和300大气压之间的压力下进行。
4.按权利要求3的方法，其中加氢处理步骤在380和420℃之间的温度和在100和180大气压之间的压力下进行。
5.按权利要求1或2的方法，其中脱沥青步骤在40和200℃之间的温度和在1和50大气压之间的压力下进行。
6.按权利要求1或2的方法，其中脱沥青步骤借助于溶剂萃取法进行。
7.按权利要求6的方法，其中溶剂是有3-6个碳原子的轻石蜡。
8.按前述权利要求的至少一个的方法，其中氢化催化剂是一种易分解的前体或基于一种或多种过渡金属的预先形成的化合物。
9.按权利要求8的方法，其中过渡金属是钼。
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Cited By (4)
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| CN100387690C (zh) * | 2000-11-30 | 2008-05-14 | 日挥株式会社 | 石油的精炼方法 |
| CN100497548C (zh) * | 2002-12-20 | 2009-06-10 | 艾尼股份公司 | 重质原料例如重质原油和蒸馏渣油转化的方法 |
| CN101558139B (zh) * | 2006-07-31 | 2013-10-16 | 艾尼股份公司 | 重质原料全部转化为蒸馏物的方法 |
| CN110607190A (zh) * | 2015-10-16 | 2019-12-24 | 沙特阿拉伯石油公司 | 从石油中除去金属的方法 |
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| IT1271473B (it) * | 1993-09-17 | 1997-05-28 | Agip Spa | Miscela idrocarburica efficace nella rimozione degli asfalteni |
-
1995
- 1995-05-26 IT ITMI951095A patent/IT1275447B/it active IP Right Grant
-
1996
- 1996-04-30 CA CA002175437A patent/CA2175437C/en not_active Expired - Lifetime
- 1996-05-01 US US08/640,506 patent/US5932090A/en not_active Expired - Lifetime
- 1996-05-14 GB GB9610091A patent/GB2301373B/en not_active Expired - Fee Related
- 1996-05-24 CN CN96107565A patent/CN1087336C/zh not_active Expired - Lifetime
- 1996-05-24 MX MX9601966A patent/MX9601966A/es unknown
- 1996-05-24 DE DE19621103A patent/DE19621103B4/de not_active Expired - Fee Related
- 1996-05-24 JP JP12971696A patent/JP3776163B2/ja not_active Expired - Lifetime
- 1996-05-27 BR BRPI9602495-0A patent/BR9602495A/pt not_active IP Right Cessation
- 1996-06-08 SA SA96170077A patent/SA96170077B1/ar unknown
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100387690C (zh) * | 2000-11-30 | 2008-05-14 | 日挥株式会社 | 石油的精炼方法 |
| CN100497548C (zh) * | 2002-12-20 | 2009-06-10 | 艾尼股份公司 | 重质原料例如重质原油和蒸馏渣油转化的方法 |
| CN101558139B (zh) * | 2006-07-31 | 2013-10-16 | 艾尼股份公司 | 重质原料全部转化为蒸馏物的方法 |
| CN110607190A (zh) * | 2015-10-16 | 2019-12-24 | 沙特阿拉伯石油公司 | 从石油中除去金属的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08319489A (ja) | 1996-12-03 |
| IT1275447B (it) | 1997-08-07 |
| ITMI951095A0 (it) | 1995-05-26 |
| GB9610091D0 (en) | 1996-07-17 |
| DE19621103A1 (de) | 1996-11-28 |
| GB2301373B (en) | 1998-09-23 |
| SA96170077B1 (ar) | 2006-05-13 |
| GB2301373A (en) | 1996-12-04 |
| CA2175437A1 (en) | 1996-11-27 |
| MX9601966A (es) | 1997-01-31 |
| DE19621103B4 (de) | 2007-09-06 |
| BR9602495A (pt) | 1998-09-08 |
| ITMI951095A1 (it) | 1996-11-26 |
| CN1087336C (zh) | 2002-07-10 |
| JP3776163B2 (ja) | 2006-05-17 |
| US5932090A (en) | 1999-08-03 |
| CA2175437C (en) | 2007-09-18 |
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