CN1098337C - 一种采用多金属液体催化剂的常压重油悬浮床加氢新工艺 - Google Patents
一种采用多金属液体催化剂的常压重油悬浮床加氢新工艺 Download PDFInfo
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Abstract
一种采用多金属液体催化剂的常压重油悬浮床加氢新工艺，主要是采用悬浮床加氢裂化反应器，并应用高分散、高活性及低成本的多金属液体催化剂；工艺中悬浮床加氢裂化反应器与固定床加氢精制反应器在线相连，以利用已存在的氢压与温度对产出的馏分油进一步加氢精制，该工艺并具有独特的催化剂分散和低温硫化设备及技术，以利于催化剂的分散和硫化；对劣质常压重油的处理具有较高的转化率和馏分油收率以及性质十分良好的石脑油、柴油产品。
Description
本发明涉及一种采用多金属液体催化剂的常压重油悬浮床加氢新工艺，它是属于石油加工工艺中的重质油轻质化工艺过程的改进。它主要是通过采用悬浮床加氢裂化反应器和具有高分散型的多金属液体催化剂，并在线使用了固定床加氢精制反应器，从而大大地提高了常压重油轻质化的收率。
世界上目前悬浮床加氢工艺研究十分活跃，现已有十多种工艺处于中试和工业示范装置阶段，个别已具备工业化条件，但这些工艺均存在着各自不足之处，例如①德国开发的VCC(VEBA-Combi-Cracking)工艺，它是采用赤泥(一种含铁的固体物或称拜尔料)及褐煤细焦粉作催化剂，该工艺不仅反应压力高(30～75Mpa)而且催化剂用量大(加入量约为原料的5％)。②美国Exxon公司开发的Micro-Cat工艺，该工艺主要用磷钼酸和环烷酸钼为催化剂，虽然催化剂的分散程度和活性均较高，但至今还停留在小试阶段(1桶/天)而且催化剂的成本很高、经济效益不高。③委内瑞纳INTEVEP公司开发的HDH工艺，它是以委内瑞纳现有的一种廉价天然矿石经粉碎和磨细后作为催化剂，虽然催化剂价格便宜，但用量也很大(2～5m％)，而且催化剂的固体物质与未转化尾油的分离系统复杂，同时该矿石仅限于该国家所特有。④加拿大的CANMET工艺，该工艺所用的催化剂是FeSO4·H2O，加入量也较大(1～5％)，同时该工艺的脱硫脱氮率不高、产品质量不够好，而且催化与未反应尾油分离上也存在问题。⑤日本旭化成工业株式会社所开发的SOC工艺，该工艺虽然采用了高分散型的超细粉末和过渡金属化合物组成的催化剂，反应活性高。抑焦效果较好，目前已建成工业示范装置，但该过程的反应压力仍然很高(20～22Mpa)，装置投资成本较高。⑥此外目前世界上还有其它工艺例如：由日本出光大产公司和美国凯罗格公司共同开发的MRH工艺；美国UOP公司开发的Aurabon工艺]；加拿大开发的(HC)3工艺等这些工艺有的处于小型试验阶段，有的催化剂用量大，有的是采用固体催化剂，有的是催化剂价格昂贵，反应压力高，而且这些工艺中大多数所用催化剂是单一催化剂或1～2种催化剂复配，而且这些工艺所加工的原料绝大多数是含硫原油，对于低硫原油渣油原料这些工艺的适应性差。
本发明的目的就在于避免上述现有技术的不足之处而提出了一种采用多金属液体催化剂的常压重油悬浮床加氢新工艺，它主要在加氢工艺上进行了多项技术创新而构成了完整的悬浮床加氢新工艺。它主要是通过在悬浮床加氢裂化反应器中使用高分散型的多金属液体催化剂，并在线地使用了固定床加氢精制反应器，从而使得该工艺既可解决低硫石油渣油，也可解决高硫石油渣油的加工，它对于含有高氮、高金属、高粘度、高酸值、高残炭的石油常减压渣油加工特别有效。其主要的技术特征是在于该工艺采用了多金属液体催化剂的悬浮床加氢裂化反应器和在线固定床加氢精制反应器，并使用了在线混合器对原料和催化剂进行充分混合和低温硫化，对反应器的流出物分别采用了高、底压分离系统和常规分离系统，对蜡油采用了回炼处理技术。所使用的工艺流程为：经充分混合并加热后的浆液由底部进入悬浮床加氢裂化反应器，反应器的顶部流出物则进入高温高压分离系统，即流出物进入热高压分器后进行分离，汽相物流进入在线固定床加氢精制反应器，而液相物流则进入低压分离系统，低压分离系统的液相物流也进入在线固定床加氢精制反应器，经固定床加氢精制后的物流最后再进入常规分离系统进行分离而得出各种产品；其中高压分离系统包括热高分器和冷高分，低压分离系统包括闪蒸罐、减压分馏塔、低压分离器、冷低分，常规分离系统包括分馏塔；其减压分馏塔中分馏出的蜡油则部分返回悬浮床加氢裂化反应器中进行回炼。
为了更好地实现本发明的上述目的，本发明的设计者是将固定床加氢精制反应器设计成在线于整个工艺流程之中，其使用的氢源来自于悬浮床加氢反应器的热物流；其用于原料和催化剂混合的在线混合器是多级剪切泵或静态混合器，多级剪切泵一般采用为2～7级剪切泵；其低压分离系统中的减压蒸馏塔的蜡油，一部分进入固定床加氢精制反应器中，另一部分随浆液一起返回悬浮床加氢反应器中，以提高柴油收率；反应器中的浆液是由循环泵不断循环以保持全返混状态；该浆液主要是由待加工渣油、液体催化剂、循环尾油、循环蜡油和新鲜氢气组成。
在上述采用多金属液体催化剂的常压重油悬浮床加氢新工艺，其悬浮床加氢裂化反应器的反应条件是反应压力为8～12Mpa，反应温度为420～460℃，总空间速度0.8～1.4，尾油/新鲜原料循环比为0.3～0.8，催化剂用量以金属计则为50～2000ppm，氢气对新鲜原料比为600～1000；在线加氢固定床反应器的反应条件是反应温度为300～400℃，压力略低于悬浮床加氢反应器的压力，空间速度为1.0～2.0，氢/油比为300～1000。悬浮床加氢裂化反应器所使用的催化剂是高分散型多金属的液体催化剂，其主要的成份是多种金属的盐类。固定床加氢精制反应器所使用的催化剂是工业上常用的3936或RN-2加氢精制催化剂。
附图的图面说明如下；
1--氢气加热炉 2--油浆加热炉 3--热高分 4--悬浮床反应器
5--闪蒸罐 6--减压蒸馏塔 7--分离器 8--固定床反应器
9--冷高分 10--冷低分 11--常压分馏塔
下面将结合附图和实施例来详叙本发明的设计思想和设计优点。
在实际设计和运行中，本发明的设计者是采用如附图所示的工艺流程，并在悬浮床加氢裂化反应器中使用了高分散型多金属液体催化剂(UPC系列)，在固定床加氢精制反应器中使用了工业上常用的3936或RN-2加氢精制催化剂。这样，原料渣油(含有高度分散催化剂和少量硫化剂)与蜡油或尾油混合被泵送至渣油加热炉，经加热至380～480℃后与加热炉出来的相应温度的氢混合，进入悬浮床加氢裂化反应器K-1。K-1出料在热高压分离器K-2中闪蒸为汽相和液相，汽相物料(包括混氢)自K-2顶部直接进入固定床在线加氢精制反应器K-3，K-2底部液流(即带有催化剂的重质油料)，经降压后进入闪蒸罐K-4进行闪蒸。K-4顶部物流与减压蒸馏塔K-5侧线物流以及分离器K-6底部物流汇合，其既可送入K-3反应器进行加氢精制，也可与分馏塔K-9塔底油混合作为蜡油出装置或与循环尾油混合经加热炉后回送入悬浮床加氢裂化反应器K-1。K-4底部液流进入减压蒸馏塔K-5，K-5塔底尾油一部分送出装置，另一部分作为尾油循环。K-5塔顶物流进入分离器K-6，K-6顶部气相作为尾气排出。固定床在线加氢精制反应器K-3的反应产物及氢气，经多次换热降温并经注水(溶解反应生成的铵盐)后进入冷高分K-7进行油、气、水三相分离。溶解了NH3，H2S的含硫污水从冷高分K-7中分出，与冷低分K-8出来的含硫污水一道送出装置统一处理。闪蒸出的冷高分气中，氢气含量较高，大部分作为循环氢经循环氢压缩机升压与新氢混合后返回反应系统。为了维持循环氢浓度达到要求，需连续排放少量冷高分气体，为减少氢耗采用膜分离器回收其中氢气，膜分离尾气送出装置进行脱硫。经冷高分K-7及冷低分K-8后的油流经换热、加热后进入常压分馏塔K-9，塔顶得到混合石脑油，侧线经汽提后得到柴油产品，塔底得到常底油与减压蒸馏塔侧线的减压蜡油混合后，作为催化裂化装置原料。
下面是按本发明的工艺流程对新疆克拉玛依常压渣油进行中试的实施例：
新疆克拉玛依常压渣油在30～100吨/年的中型装置上反应温度为400～480℃；氢分压4～12Mpa，采用UPC-21多金属液体催化剂；总原料空速1.0～1.3h-1，新鲜原料空速0.4～0.8h-1，悬浮床加氢裂化＜524℃收率达90～97m％。具体数据如下：1.克炼常渣在不同反应温度下悬浮床加氢裂化的产物分布(单程收率)：
2.克炼常渣在不同反应温度下悬浮床加氢的产物分布(单程及循环收率)：
3.精制前后石脑油馏分(IBP～180℃)组成与性质：
4、精制前后柴油馏分(180～350℃)组成与性质
| 反应温度，℃ | 430 | 435 | 440 | 445 | 450 |
| 氢分压，Mpa | 10.0 | 10.0 | 10.0 | 10.0 | 10.0 |
| 氢油比，Mm3/m3 | 740/1 | 742/1 | 757/1 | 737/1 | 735/1 |
| 总体积空速，1/h | 1.13 | 1.13 | 1.10 | 1.13 | 1.14 |
| 产物分布，m％C1-C4(气体)收率C5～180℃(石脑油馏分)收率180～350℃(柴油馏分)收率350～524℃(蜡油馏分)收率＜524℃收率＞524℃(尾油)收率氢耗，m％总收率，m％ | 4.636.6719.0239.8970.2130.841.06101.6 | 4.707.9722.5639.5175.1326.061.09101.19 | 4.769.2724.0837.5075.6125.391.13101.0 | 4.9610.2827.4137.6280.2720.901.18101.18 | 5.0311.6830.5535.0082.2519.001.25101.25 |
| 反应温度，℃ | 440 | 440 | 445 | 445 |
| 氢分压，Mpa | 10.0 | 10.0 | 10.0 | 10.0 |
| 氢油比，Mm3/m3 | 757/1 | 800/1 | 737/1 | 800/1 |
| 循环比(新鲜原料/尾油) | 100 | 66/34 | 100 | 70/30 |
| 总体积空速，1/h | 1.10 | 1.14 | 1.13 | 1.14 |
| 新鲜原料体积空速，1/h | 1.10 | 0.75 | 1.13 | 0.80 |
| 产物分布(占新鲜原料)，m％C1-C4(气体)收率C5～180℃(石脑油馏分)收率180～350℃(柴油馏分)收率350～524℃(蜡油馏分)收率＜524℃收率＞524℃(尾油)收率氢耗，m％总收率，m％ | 4.769.2724.0837.5075.6125.391.13101.0 | 5.509.6027.3053.1096.304.600.92100.92 | 4.9610.2827.4137.6280.2720.901.18101.18 | 7.4013.8029.6045.4096.205.001.18101.18 |
| 精制条件 | 精制前 | 精制后 | 精制后 | 精制后 | 精制后 |
| 精制原料馏分组成，℃ | -- | IBP～350 | IBP～350 | IBP～350 | IBP～500 |
| 精制温度，℃ | -- | 360 | 380 | 400 | 400 |
| 精制压力，MPa | -- | 10.0 | 10.0 | 10.0 | 10.0 |
| 烃族组成，m％ | |||||
| 正构烷烃 | 20.61 | 24.94 | 24.97 | 25.05 | 21.30 |
| 异构烷烃 | 32.81 | 38.04 | 38.95 | 39.62 | 36.50 |
| 环烷烃 | 15.91 | 31.63 | 31.34 | 30.97 | 33.65 |
| 芳香烃 | 10.40 | 5.39 | 4.74 | 4.36 | 6.10 |
| 烯烃 | 20.27 | 0.0 | 0.0 | 0.0 | 0.0 |
| 芳烃潜含量，m％ | - | 38～42 | 38～42 | 38～42 | 38～42 |
| 辛烷值 | 78.1 | 73.4 | 73.9 | 74.3 | 75.0 |
| 密度(20℃)，g/cm3 | 0.7543 | 0.7451 | 0.7454 | 0.7519 | 0.7499 |
| 硫，μg/g | 440 | 0.5～1.0 | 0.5～1.0 | 0.2～0.6 | 0.5～1.0 |
| 氮，μg/g | 658 | 1.0～2.0 | 1.0～2.0 | 0.5～1.5 | 1.0～2.0 |
| 碱性氮，μg/g | 160 | ＜1.0 | ＜1.0 | ＜1.0 | ＜1.0 |
| 项目 | 精制前 | 精制后 | 精制后 | 精制后 | 精制后 |
| 精制原料馏分组成，℃ | - | IBP～350 | IBP～350 | IBP～350 | IBP～500 |
| 精制温度 | - | 360℃ | 380℃ | 400℃ | 400℃ |
| 精制压力，Mpa | - | 10.0 | 10.0 | 10.0 | 10.0 |
| 密度(20℃)，g/cm3 | 0.8464 | 0.8303 | 0.8241 | 0.8202 | 0.8449 |
| 粘度(20℃)，mm2/s | 8.79 | 3.83 | 3.47 | 3.40 | 3.97 |
| 粘度(40℃)，mm2/s | 3.16 | 2.70 | 2.33 | 2.18 | 2.58 |
| 硫，μg/g | 570 | 18.2 | 13.5 | 12.4 | 19.3 |
| 氮，μg/g | 1510 | 5.5 | 4.3 | 4.1 | 8.9 |
| 碱性氮，μg/g | 780 | 5.0 | 3.9 | 3.6 | 5.9 |
| 苯胺点，℃ | 62.2 | 72.0 | 72.0 | 70.1 | 67.9 |
| 十六烷值 | 49.6 | 58.1 | 60.3 | 62.2 | 53.1 |
| 酸度，mgKOH/100ml | 35.62 | 3.40 | 2.1 | 2.14 | 3.45 |
| 凝点，℃ | -38 | -37 | -37 | -32 | -37 |
| 冷滤点，℃ | ＜-20 | ＜-20 | ＜-20 | ＜-20 | ＜-20 |
本发明的加氢裂化工艺与现有技术中的各类加氢裂化工艺的不同点在于：
(1)本工艺的悬浮床加氢裂化反应器采用高度分散(微米或纳米级)的多金属液体催化剂(催化剂的有效金属组分包括镍、铁、钼、锰、钴等)，催化剂中金属组分相当一部分系来自工业废料中回收得到，因而成本大大降低。这与世界上常用的固体粉末催化剂或组分较少的分散型催化剂有根本区别。
(2)本工艺的另一特点是采用独特的催化剂分散和低温硫化技术，原料油与催化剂在流动管路中采用2～4级剪切泵，在转速为2000～5000转/分下进行分散混合，并在100～180℃温度下和含有硫化氢的气体中完成混合料中催化剂的硫化。
(3)与世界上同类工艺不同，本工艺采用以蜡油或尾油的循环裂化路线，装置主要产物是石脑油和柴油以及少量尾油。
(4)由于本工艺采用全返混式裂化反应器，少量焦炭不会沉降，反应器温度十分均匀易于控制，从而简化了反应器操作及温度控制。同时由于本发明采用高温、高压在线加氢精制反应器，不仅充分地利用了已有的反应温度和压力，而且使产物性质十分优良。
与现有技术相比，本发明具有以下优点：
(1)由于本发明采用多金属液体催化剂具有高分散性能，催化剂粒度小(0.1～5微米)、活性高、用量少(用量低于0.1％)加之催化剂中许多金属组分来自工业废料因而成本低，每加工一吨渣油催化剂成本在20～30元(人民币)。
(2)由于催化剂高活性因而反应温度高(430～460℃)，裂化转化率高(80～96％)，生焦量少(＜1％)。
(3)反应压力低(反应氢分压为8～12.0Mpa)，工业流程简单(1-2个反应器)，装置建设投资成本低。
(4)由于采用全返混裂化反应器和蜡油循环裂化及高温高压在线精制反应器，不仅不需再建加氢精制和蜡油加氢裂化装置，而且产品质量高(石脑油可作重整原料及裂解原料，柴油为高十六烷值、低硫、低氮优质柴油)。
(5)由于采用蜡油或尾油循环，大大增加该装置操作灵活性，使该工艺以生产石脑油和柴油为主，需要时也可生产蜡油。
本发明的工艺方法，可起到“一顶四”的特殊效用，即使用本发明的工艺装置，可以对走加氢路线的加工方案在达到同样收率的前提下省略掉减压分馏塔、催化裂化、减压渣油加氢裂化和加氢精制四套处理装置。对处理各种劣质重油及稠油包括辽河、孤岛和新疆稠油的常压渣油及特稠原料都有十分明显的效果，尤其是对于含高氮、高金属、高粘度、高酸值和高残碳的石油常压渣油的加工处理特别有效，其转化率可达80～95％以上。因此具有极大的推广应用前景。
Claims (8)
1.采用多金属液体催化剂的常压重油悬浮床加氢工艺，它主要是采用悬浮床反应器和在线固定床反应器与产物分离系统相结合的方法，其特征在于该工艺采用了多金属液体催化剂的悬浮床加氢裂化反应器和在线固定床加氢精制反应器，并使用了在线混合器对原料和催化剂进行充分混合和低温硫化，对反应器的流出物分别采用了高、底压分离系统和常规分离系统，对蜡油采用了回炼处理技术；该悬浮床加氢裂化反应器的反应条件是反应压力为8～12Mpa，反应温度为420～460℃，总空间速度0.8～1.4，尾油/新鲜原料循环比为0.3～0.8，催化剂用量以金属计则为50～2000ppm，氢气对新鲜原料比为600～1000；在线加氢固定床反应器的反应条件是反应温度为300～400℃，压力略低于悬浮床加氢反应器的压力，空间速度为1.0～2.0，氢/油比为300～1000。
2.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述工艺流程为：经充分混合并加热后的浆液由底部进入悬浮床加氢裂化反应器，反应器的顶部流出物则进入高温高压分离系统，即流出物进入热高压分器后进行分离，汽相物流进入在线固定床加氢精制反应器，而液相物流则进入低压分离系统，低压分离系统的液相物流也进入在线固定床加氢精制反应器，经固定床加氢精制后的物流最后再进入常规分离系统进行分离而得出各种产品；其中高压分离系统包括热高分器和冷高分，低压分离系统包括闪蒸罐、减压分馏塔、低压分离器、冷低分，常规分离系统包括分馏塔；其减压分馏塔中分馏出的蜡油则部分返回悬浮床加氢裂化反应器中进行回炼。
3.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述的固定床加氢精制反应器是在线于整个工艺流程之中，其氢源来自于悬浮床加氢反应器的热物流。
4.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于用于原料和催化剂混合的在线混合器是多级剪切泵或静态混合器。
5.根据权利要求4所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述的多级剪切泵为2～7级剪切泵。
6.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述的低压分离系统中的减压蒸馏塔的蜡油，一部分进入固定床加氢精制反应器中，另一部分随浆液一起返回悬浮床加氢反应器中，以提高柴油收率。
7.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述的悬浮床加氢裂化反应器是全返混式反应器，反应器中的浆液是由循环泵不断循环以保持全返混状态；该浆液主要是由待加工渣油、液体催化剂、循环尾油、循环蜡油和新鲜氢气组成。
8.根据权利要求1所述的一种采用多金属液体催化剂的常压重油悬浮床加氢工艺，其特征在于所述的悬浮床加氢裂化反应器所使用的催化剂是高分散型多金属的液体催化剂，其主要的成份是多种金属的盐类。
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| US6660157B2 (en) | 2003-12-09 |
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