CN1164867A - 从烃油中除去环烷酸的方法 - Google Patents

从烃油中除去环烷酸的方法 Download PDF

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CN1164867A
CN1164867A CN95195221.8A CN95195221A CN1164867A CN 1164867 A CN1164867 A CN 1164867A CN 95195221 A CN95195221 A CN 95195221A CN 1164867 A CN1164867 A CN 1164867A
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K·格兰德
C·索莱
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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
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
    • C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/107—Atmospheric residues having a boiling point of at least about 538 °C

Abstract

从尚未经蒸馏为馏分的原油或是仅蒸去石脑油馏分的原油中去除环烷酸的方法是：原油于1～50bar、100～300℃下于一种与常压残油加氢所用同类的催化剂上加氢，该催化剂优选含镍—钼或钴—钼且沉积于氧化铝载体材料上。

Description

从烃油中除去环烷酸的方法
本发明涉及一种从烃油中去除环烷酸的方法，尤其是从尚未经蒸馏为馏分的原油或是仅蒸去石脑油馏分的原油中去除。
众所周知，原油及原油馏分中含硫化合物、氮化合物和其它不希望存在的化合物，为从原油馏分中去除这类化合物，已提出了许多方法，催化加氢是非常常用的一种去除硫、氮组分的方法。石脑油馏分加氢时典型的操作压力为10～30bar，温度为250～400℃；另外，残油的处理在100～150bar下进行，温度为35～450℃。这种加氢处理还可去除烃馏分中所含的任一种环烷酸。此处环烷酸一词用作环烷酸、芳香酸以及石蜡族羧酸的通称。
由于环烷酸对过程设备具有很强的腐蚀作用，故人们常常亟待从烃油中有针对地除去环烷酸。为此，在石油精制过程中尽可能早地除去环烷酸是有益的。
现已发现进行这种环烷酸除去的可能的方法，即在非常温和的条件下，通过对环烷酸的选择性加氢，从而从未分馏的或是仅经拨头处理的原油中将其除去。在如此温和条件下，可避免大量的脱硫反应、脱氮反应以及可导致芳香烃饱和的反应，故此可保证氢的耗量适度。
所以，本发明提供一种从烃油中除去环烷酸的方法，在该法中，烃油于催化剂上经高温加氢，所用催化剂类型与常压残油加氢时所用者相同，优选催化剂含镍-钼或是钻一钼且沉积在氧化铝载体材料上。该法的特征在于，所用烃油为
(a)尚未经蒸馏为馏分的原油，或是
(b)已蒸去石脑油馏分的原油；和，加氢在20～30bar、100～300℃下进行。
本发明方法的两实施方案中，进行加氢的优选条件是：20～30bar，温度200～250℃。
所述加氢宜于一个或数个并置的带有固定催化剂床的反应器内进行。如上言及，本发明方法所用催化剂为在常压残油加氢中行之有效的一类催化剂。实施本发明方法成功的关键是催化剂载体材料孔率充分大，以期使原油中最重的组分也可穿过并进入催化剂的孔道。因而，载体材料的孔率应可使最终担载后的催化剂的孔率优选在10～12nm(纳米)的量值。优选使用的催化剂含镍-钼或是钴-钼且沉积于氧化铝载体材料上。油流过催化剂的流率优选为0.5至5.0m3油/(m3催化剂·小时)，更优选为1.0～3.0m3油/(m3催化剂·小时)。
作为原油的预处理，适宜以水对原油进行常规的脱盐。
本发明方法可使原油中环烷酸组分的选择性降低到约5％～6％以下，与此同时，可能存在的硫化合物及氮化合物不会被氢化。随着环烷酸含量的大幅降低，原油中的金属含量也随之产生一定程度的减小。这并无害处；尤其是对那种在诸如催化裂化器内进行加工的加氢原油更是如此，原因在于用作加氢过程的催化剂较之用在裂化过程中的催化剂对金属具有更高的耐受性能。故此，如若对原油进行裂化，宜于足够高的温度下实施本发明的方法，以求甚而是金属含量大大减少，而不论如此高温会导致硫、氮含量的大大降低及随之而来的氢耗量增加，可能还有必要回收硫且脱氮。
本发明方法易于与原油精炼方法配套用于酸性原油精炼、一俟原油经除盐且通过热交换加热至100～300℃(优选值230～250℃)，则将该原油通入一实施本发明方法的加氢反应器系统，继之通入精炼系统的下一个热交换器，再而进入原油再沸器，最后通入蒸馏塔。较之先有的那些更为苛刻的原油加氢处理而言，由本发明方法所取得的有效而温和的环烷酸加氢限定了氢在原油精炼过程中的耗量，因之也降低了加氢反应器的成本。使本发明方法与精炼方法配套的成本仅为一个传统的成套预处理工厂的一小部分。因而，如若将该新方法与原油精炼方法合并，则无需任何附加除盐器、热交换器及汽提器，也不需对废水处理额外增容。
以下将举例详述本发明方法的实施方案。该实施方案的主要特征示于附图中。
将引自库存的原油加热到100～150℃并于其内加入新鲜水。水与原油的混合物泵至除盐器，在重力及外加电场作用下，器内混合物分离为油和水。含盐水尚含少量烃，遂送至水净化厂。除盐后的原油通过预分馏装置，在该装置内，油中约15％的最轻质组分得以分离，该馏分为一种沸点高达100～200℃的石脑油馏分。这种预分馏并非绝对必要，但对改善随后的加氢操作条件有利，原因是该处理减小了烃的分压以及通过加氢装置的总体积流率。
由预分馏装置引出的底端馏分泵至加氢装置，于此它先与所述加氢装置引出的富氢循环气以及来自氢气工厂的新鲜配料氢气混合，氢气工厂可以是对天然气、LPG或石脑油进行蒸汽预转化的工厂。混合后的原料随之加入5个并行设置的反应器，每一反应器均具有固定的催化剂床层，其中催化剂含载于Al2O3上的Ni-Mo。一旦与催化剂接触，则原油中的羧基(尤其是环烷酸的羧基)就与氢反应并生成水。加氢反应器的流出物通入高压分离器，该分离器产生的液体再通入低压分离器，而高压分离器引出的气体则如前述循环作为原料。如有必要，从低压分离器分离出的气体可同取自前述循环气的吹扫物流一加通入硫回收工厂。从低压分离器引出的原油通入汽提塔，于此最轻质烃及全部H2S均被汽提出来。如必要，这部分气流也可通入硫回收工厂。从汽提塔引出的经处理后的原油再与加氢前于预分馏装置中原油中分离出的拔头馏分混合，所得混合物送至中和油贮槽。
实施本发明方法适宜的设备及流程与周知的汽油加氢方法中所采用者基本类同，但有例外的是，对本方法，一般并不需要与回收硫和脱氮有关的设备。熟悉本领域的人不难使公知的汽油加氢技术与本发明方法结合。
本发明更详尽地体现在如下实施例中。
实施例1
在一加氢中试工厂里，使用以固定床方式填充500mL催化剂的反应器，对0.SL/h的原油进行加氢。试验进行若干次，压力为20bar，温度分别为230，250，300及350℃。催化剂为载于Al2O3上的镍-钼，其孔尺寸为10～12纳米。H2用量为每升油200标准升H2，每升催化剂每小时流过催化剂的油量为1升。未经处理的原油的性能如下：
酸值，mg KOH/g油    2.6
金属含量，ppm       10
硫含量，ppm         4572
氮含量，ppm         541
相应酸值减小所得结果列于下表1，其中也给出了加氢后原油的金属含量、硫含量以及氮含量。
表1
 温度℃ 酸值mg KOH/g  金属含量ppm 硫含量ppm 氮含量ppm
  230     0.15     7.5     4572     542
  250     0.07     5.5     4334     525
  300     0.06     4.2     3019     510
  350     0.15     2.9     1452     506
试验结果表明，在230℃、20bar下可选择性氢化原油中的环烷酸，并使酸值为2.6mg KOH/g油的油降为0.15mg KOH/g油的油。在可测定范围内，原油中的硫化合物及氮化合物并未氢化，故此可以推断，所述加氢可以商用规模进行而无需进行硫回收和脱氮。随酸值的大幅降低，甚而原油中的金属含理也于230℃下有一定程度减小，即由10ppm降至7.5ppm。这并无害处，尤其是对于那种在诸如催化裂化器内进行加工的氢化原油更是如此，原因在于用作加氢过程的催化剂较之用在裂化过程中的催化剂对金属具有更高的耐受性能。
即使在更高温度下，即250、300及350℃，所获酸值减小也极会令人满意，而且金属含量的减小也更大。但是，随温度增加，硫化合物及氮化合物的氢化也会增大，这会增大氢的耗量且有必要回收硫和脱氮，这对本发明方法而言是最不希望发生的事。
取上述未经处理的原油在230℃下进行试验，条件也同前述，结果表明：以总酸值(单位mg KOH/g)表示的催化剂稳定性在对其性能进行考察的长时间内几乎保持为常数，这对商用操作是有利的。所得结果在下表2中给出。
表2
     230℃下催化剂的稳定性
   运行天数   总酸值(mg KOH/g)
    1     0.1
    10     0.2
    40     0.2
    60     0.2
    95     0.2
原油酸值减小至0.5mg KOH/g以下可视为足以达到本发明的目标。
实施例2
除操作压力增至50bar外，进行试验的其它条件均与实施例1中相同。
相应酸值减小所得结果列于下表3，其中也给出了加氢后原油的金属含量、硫含量以及氮含量。
表3
 温度℃  酸值mg KOH/g 金属含量ppm 硫含量ppm 氮含量ppm
  230     0.15     7.8     4468     558
  250     0.07     5.9     4270     539
  300     0.06     3.1     3102     524
  350     0.39     1.3     1176     481
即使是原油在50bar下氢化时，在230℃下也可达到酸值大幅减小，同样金属含量也由10ppm降至7.8ppm。随温度升高结果的变化趋势与实施例1中在20bar下氢化的结果大体相同。

Claims (10)

1.从烃油中除去环烷酸的方法，其中烃油在高温下于一种与常压残油加氢所用同类的催化剂上加氢，该催化剂优选含镍-钼或钴-钼且沉积于氧化铝载体材料上，而且其中所用烃油为a)尚未经蒸馏为馏分的原油或是b)己蒸去石脑油馏分的原油，且加氢在1～50bar、100～300℃下进行。
2.按照权利要求1的方法，其特征在于加氢在1～50bar、100～300℃下进行。
3.按照权利要求1或2的方法，其特征在于所用催化剂的孔率介于10至20nm(纳米)间。
4.按照权利要求1至3任一项的方法，其特征在于所述原油的加料流率为每小时每m3催化剂0.5～5.0m3油。
5.按照权利要求4的方法，其特征在于原油的加入流速率为每小时每m3催化剂1.0～3.0m3油。
6.按照权利要求1至5任一项的方法，其特征在于所用原油已经除盐。
7.按照权利要求1至6任一项的方法，其特征在于它在1个或多个具有固定催化剂床的反应器内进行的。
8.按照权利要求1至7任一项的方法，其特征在于所用原油需经精炼加工，它先经除盐并加热至100～300℃，优选230～250℃，加氢后再循环至精炼过程中进一步加热，再加入蒸馏塔中。
9.按照权利要求1至8任一项的方法，其特征在于所用原油已蒸去石脑油馏分且该馏分与加氢后的原油混合。
10.按照权利要求1至9任一项的方法，其特征在于加氢在足够高温度下进行，以使甚而是原油中的金属含量及硫含量也得大幅降低。
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MX9701483A (es) 1998-02-28
ATE187197T1 (de) 1999-12-15
EP0778873B1 (en) 1999-12-01
CA2198623A1 (en) 1996-03-07
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AU3534695A (en) 1996-03-22
DE69513669T2 (de) 2000-04-06
DE69513669D1 (de) 2000-01-05
WO1996006899A1 (en) 1996-03-07
CN1051569C (zh) 2000-04-19
ES2139242T3 (es) 2000-02-01
NO943188L (no) 1996-03-01

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