CN101027127A - 高活性浆液催化剂组合物 - Google Patents

高活性浆液催化剂组合物 Download PDF

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CN101027127A
CN101027127A CNA2005800303569A CN200580030356A CN101027127A CN 101027127 A CN101027127 A CN 101027127A CN A2005800303569 A CNA2005800303569 A CN A2005800303569A CN 200580030356 A CN200580030356 A CN 200580030356A CN 101027127 A CN101027127 A CN 101027127A
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carbon monoxide
olefin polymeric
reaction zone
slurries
mixture
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CN101027127B (zh
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陈开东
B·E·雷诺兹
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Chevron USA Inc
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Abstract

本发明涉及浆液催化剂组合物的制备。所述浆液催化剂组合物以一系列步骤制备，包括使VIB族金属氧化物和氨水混合形成含水的混合物和硫化所述混合物从而形成浆液。然后用VIII族金属促进所述浆液。后续步骤包括将所述浆液与烃油混合，然后将得到的混合物与氢气合并(在使水保持液相的条件下)生成所述活性浆液催化剂。

Description

高活性浆液催化剂组合物
发明领域
本发明涉及用于重油加工的浆液催化剂组合物的制备。这些重油的特征在于氢碳比低，而炭渣、沥青质、氮、硫和金属含量高。
发明背景
浆液催化剂组合物和其制备方法在炼油领域中是已知的。下文讨论一些实例。
美国专利No.4,710,486公开了一种制备分散的VIB族金属硫化物烃油加氢处理催化剂的方法。该方法的步骤包括氨水和VIB族金属化合物(如氧化钼或氧化钨)反应形成水溶性的含氧化合物，如钼酸铵或钨酸盐。
美国专利4,970,190公开了一种制备用于烃油加氢处理的分散性VIB族金属硫化物催化剂的方法。该催化剂用VIII族金属促进。该方法的步骤包括用氨水溶解VIB族金属化合物(如氧化钼或氧化钨)形成水溶性的化合物，如含水的钼酸铵或钨酸铵。
美国专利Nos.5,164,075和5,484,755(在后专利引入作为参考)公开了由VIB族金属化合物制备用于加氢处理重烃油类的高活性浆液催化剂的方法。金属化合物的含水混合物用每磅VIB族金属大于约8至约14标准立方英尺的硫化氢硫化。这些专利公开了一种形成浆液催化剂前体然后将该前体加入重原料油中形成活性催化剂的方法。但是，这些专利未说明形成高活性催化剂组合物时油粘度的关键性，也未说明在关键反应阶段中将水保持液相的重要性。
在美国专利Nos.5,164,075和5,484,755中公开的发明无法形成油水乳剂或浆液相，导致形成了钝化的催化剂或活性低的催化剂。
本申请公开了一种新的高活性浆液催化剂组合物。使用在212具有合适粘度范围的单一烃油(优选减压瓦斯油)制备所述催化剂产生了该活性。
发明概述
本发明涉及适于加工重烃油类的高活性催化剂组合物。所述催化剂通过下列步骤制备，得到适用于加氢转化重油的催化剂组合物，该催化剂通过下述步骤制备：
(a)将VIB族金属氧化物和氨水混合形成VI族金属化合物的含水混合物；
(b)在最初反应器中，用含有硫化氢的气体硫化步骤(a)的含水混合物至加药量大于8 SCF硫化氢每磅VIB族金属，形成浆液；
(c)用VIII族金属化合物促进浆液；
(d)将步骤(c)的浆液与具有至少2 cSt(或32.8 SSU)@212粘度的烃油混合形成混合物X；
(e)混合物X与氢气在第二反应区中在将混合物X中的水保持液相的条件下合并，形成与液态烃混合的活性催化剂组合物；和
(f)回收活性催化剂组合物。
这种新的高活性浆液催化剂组合物可以活性的和浓缩的状态储存。该催化剂组合物可以直接引入任何已知的重油或残油改质的工艺过程中，引入的条件是这些工艺过程中存在的条件。该催化剂可以在稀释或不稀释原料的同时改质粘度很高的含碳的和/或高链烷原料。
附图说明
附图说明了涉及制备该催化剂组合物的步骤。
发明详述
本发明涉及新的高效浆液催化剂组合物，其通过混合含有VIB族和VIII族金属的浆液和具有至少2 cSt(或32.8 SSU)@212粘度的烃油形成。烃油优选的粘度范围是从至少约2 cSt(或32.8 SSU)@212到15 cSt(或77.9 SSU)@212。附图说明了本发明方法涉及的步骤。所述活性浆液催化剂组合物通过将管线5输送的VIB族金属(如钨或钼)氧化物和管线7输送的氨水在混合区10中混合而制备。混合区的温度通常在约80至约200，优选约100至约150，最优选约110至约120。混合区10的压力通常为常压至约100psig，优选约5psig至约35psig，最优选约10psig至约35psig。VIB族金属氧化物溶于含氨的水中。氨的加入量基于NH3对VIB族氧化物的比以磅/磅计，通常为0.1磅/磅至约1.0磅/磅，优选约0.15磅/磅至约0.50磅/磅，最优选约0.2磅/磅至约0.30磅/磅。在氨水中溶解的金属氧化物经管线15输送至第一反应区。
硫化氢(管线9)加入到反应区20的量基于H2S对VIB族金属氧化物的比以SCF/磅计，通常范围在4.0 SCF/磅至约20 SCF/磅，优选约8.0SCF/磅至约18 SCF/磅，最优选约12 SCF/磅至14 SCF/磅。在第一反应区内的反应时间范围为每磅VIB族金属氧化物约1小时至10小时，优选3小时至8小时，最优选约4小时至6小时。条件包括温度范围为80至200，优选100至180，最优选130至160。压力范围为100至3000psig，优选200至1000psig，最优选300至500psig。产物浆液是在含水浆液相中的催化剂前体。
如美国专利No.5,484 755所公开的，将产物浆液与VIII族金属化合物(如Ni或Co)结合。作为本发明活性浆液催化剂脱氮活性的增强剂，优选在将浆液与原料油和含氢的气体在高温和高压下混合前，将VIII族金属化合物加入到所述浆液中。这种VIII族金属例如是镍和钴。优选镍或钴对钼的重量比范围为约1∶100至约1∶2。最优选镍对钼的重量比范围是约1∶25至1∶10，即，促进剂占钼的4-10wt％。所述VIII族金属，例如镍，通常以硫酸盐的形式加入，优选在浆液硫化后，在pH约10或更低、优选pH约8或更低将其加入所述浆液。也可使用VIII族金属硝酸盐、碳酸盐或其它的化合物。鉴于本发明浆液催化剂的高活性，通过用VIII族金属化合物进一步促进是非常有益的。
含VIII族金属促进剂的浆液经管线25输送至混合区30。混合区30使用惰性气氛，其可以包括氮气、炼厂气、或任何其它含有很少或不含氧气的气体。所述浆液和烃油(管线11)(如VGO)以高剪切模式在混合器30中连续混合以保持浆液均质。高剪切混合包括100至1600RPM。优选混合速度大于500 RPM，最优选大于1500 RPM。
烃油具有至少2 cSt(32.8 SSU)@212的动力粘度。动力粘度通常可以是至少约2 cSt(32.8 SSU)@212至约15 cSt(77.9 SSU)@212，优选约4 cSt(39.5 SSU)@212至约10 cSt(59.2 SSU)@212，最优选约5 cSt(42.7 SSU)@212至约8 cSt(52.4 SSU)@212。所述烃油导致催化剂前体从水基初步转化成油基。VIB族金属氧化物对油的比至少小于1.0，优选小于0.5，更优选小于0.1。如果油的动力粘度低于约2 cSt(32.8 SSU)@212或大于约15 cSt(77.9 SSU)@212，催化剂前体的第一次转化将导致催化剂颗粒聚结或相反无法混合。这种混合物在权利要求中称为混合物X。
所述物料从混合区30(混合物X)经管线35输送到反应区40。将氢连续加入到反应区40的混合物中，在反应区40中采用高剪切混合以使其保持为均质浆液。在进入反应器40前，氢在低压下加入，在反应器40后，氢在高压下加入。这样操作是为了在反应器40中将水保持在液相中，在反应器40后将水转化为气相，从而闪蒸出水。当在反应器40中使用低H2速度时，水仍然在液相中。在反应器40后，加入更多的H2，从而使水转化为气相，使其在高压分离器中与油浆分离。反应器40的工艺条件是形成最终催化剂的关键。混合物中的水必须保持在液相中。
反应区40的温度通常在300至600，优选约350至约500，最优选350至450。反应区40的压力范围通常为约100至约3000psig，优选约200psig至约1000psig，最优选约300psig至约500psig。加入反应区40的氢气流量范围通常为约300 SCFB至约2000SCFB，优选约300SCFB至约1000 SCFB，最优选约300 SCFB至约500 SCFB。反应区40的反应时间范围为约10分钟至5小时，优选30分钟至3小时，最优选约1小时至1.5小时。所述产物浆液混合物是与烃油混合的活性催化剂组合物。
所述浆液混合物通过管线55输送至高压分离器50。在管线55加入更多氢气，从而将水转换为气相。然后可以在高压分离器中使水与油浆分离。高压分离器在300至700操作。气和水经管线45从塔顶除去，然后被送至三相分离器。活性催化剂组合物经管线65送至储槽60。活性催化剂组合物在储槽60中连续地混合以在含很少或没有氧气的氢气气氛下保持为均质浆液。用这种方法，保持催化剂活性和稳定性。
所述催化剂组合物用于提高含碳原料的等级，含碳的原料包括常压瓦斯油、减压瓦斯油、脱沥青油、烯烃、从焦油砂矿或沥青得到的油、从煤得到的油、重质原油、费-托法得到的合成油和从再循环油废料和聚合物得到的油。所述催化剂组合物非限制性地用于氢化提高等级的工艺过程，如热加氢裂化、加氢处理、加氢脱硫、加氢脱氮和加氢脱金属。
                         实施例
                 实施例1：催化剂的制备
540克MoO3与79克NH3和2381克水混合形成总量3000克的溶液。然后通过将在H2中含20％H2S的气体混合物在强混合作用下通入所述溶液，使所述溶液与10.71 SCF的H2S反应。反应器温度是150，总压力是400psig，反应时间是4小时。反应后，将含36克Ni的460克NiSO4溶液加入到上述得到的浆液。得到的浆液混合物然后与8000克减压瓦斯油在100混合。VGO的粘度是5 cSt@212。然后将得到的混合物与氢气连续地泵入连续流罐式反应器(优选混流反应器)。H2气体流量是300SCF/B。所述反应器压力是400psig，反应器温度是400，总反应时间是1小时。所述反应产物与更多的、气体流量为1500 SCF/B的H2混合，然后进入热的高压分离器，保持压力在400psig以及温度在500下使气体液体浆液分离。得到的液体浆液含高活性催化剂成分。

Claims (16)

1.适用于重油加氢转化的催化剂组合物，其通过下述步骤制备：
(a)使VIB族金属氧化物和氨水混合形成VI族金属化合物含水混合物；
(b)在最初的反应器中，用含有硫化氢的气体硫化步骤(a)的含水混合物至加药量大于8 SCF硫化氢每磅VIB族金属，以形成浆液；
(c)用VIII族金属化合物促进浆液；
(d)使步骤(c)的浆液与具有至少2 cSt @212粘度的烃油混合形成混合物X；
(e)混合物X与氢气在第二反应区在使混合物X中的水保持液相的条件下合并，从而形成与液态烃混合的活性催化剂组合物；和
(f)回收所述活性催化剂组合物。
2.权利要求1的催化剂组合物，其中第一反应区的条件包括温度范围为至少约80至约200，压力范围为至少约100psig至约3000psig。
3.权利要求2的催化剂组合物，其中第一反应区的条件包括温度范围为至少约100至约180，压力范围为至少约200psig至约1000psig。
4.权利要求3的催化剂组合物，其中第一反应区的条件包括温度范围为至少约130至约160，压力范围为至少约300psig至约500psig。
5.权利要求1的催化剂组合物，其中烃油的粘度范围为至少2 cSt@212至约15 cSt @212。
6.权利要求1的催化剂组合物，其中步骤(c)的VIII族金属化合物选自硫酸镍和硫酸钴。
7.权利要求1的催化剂组合物，其中成分的混合以高剪切模式进行，范围为100RPM至1600RPM。
8.权利要求6的催化剂组合物，其中镍或钴对钼的重量比范围为1∶100至约1∶2。
9.权利要求1的催化剂组合物，其中VIB族金属氧化物对油的比至少小于1.0，优选小于0.5，更优选小于0.1。
10.权利要求1的催化剂组合物，其中所述烃油是减压瓦斯油。
11.权利要求1的催化剂组合物，其中第二反应区的条件包括温度范围为至少约350至约600，压力范围为至少约100psig至约3000psig。
12.权利要求11的催化剂组合物，其中第二反应区的条件包括温度范围为至少约350至约600，压力范围为至少约200psig至约1000psig。
13.权利要求12的组合物，其中氢气连续地加入到第二反应区，使用高剪切混合以保持浆液匀质。
14.权利要求1的催化剂组合物，其通过高压分离器回收。
15.权利要求1的催化剂组合物，其以活性的和浓缩的状态储存。
16.权利要求14的催化剂，其在储槽中连续混合以保持浆液匀质。
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EA011428B1 (ru) 2009-02-27
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US20060058174A1 (en) 2006-03-16
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