CN114729273B - 制备航空燃料组分的方法 - Google Patents

制备航空燃料组分的方法 Download PDF

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CN114729273B
CN114729273B CN202080082536.6A CN202080082536A CN114729273B CN 114729273 B CN114729273 B CN 114729273B CN 202080082536 A CN202080082536 A CN 202080082536A CN 114729273 B CN114729273 B CN 114729273B
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atmospheric pressure
feedstock
weight
fraction boiling
stream
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CN114729273A (zh
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乌拉·基斯基
萨拉·利坎德
卡蒂·桑德伯格
皮尔霍·塞科宁
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Neste Oyj
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Abstract

本发明涉及用于由包含化石加氢处理进料和第二进料的原料(10)制备航空燃料组分(80)的方法，所述第二进料包含脂肪酸和松香的酯、游离脂肪酸和树脂酸。所述方法包括使原料经受加氢处理反应条件以产生经加氢处理的流(20)，将经加氢处理的流分离成三个馏分(30、40、50)，其中使至少部分最高沸点馏分(50)经受加氢裂化反应以产生经加氢裂化的流(60)。将至少部分经加氢裂化的流与至少部分经加氢处理的流混合，并将它们的混合物(70)进一步加工直到获得原料向航空燃料组分的所需转化。

Description

制备航空燃料组分的方法
技术领域
本发明涉及用于由包含化石加氢处理进料(fossil hydrotreatment feed)和第二进料的原料制备航空燃料组分的方法，所述第二进料包含脂肪酸和松香的酯(esters offatty acids and rosins，脂肪酸酯和松香酯)、游离脂肪酸和树脂酸(resin acid)。
背景技术
由于减少温室气体排放的全球举措，预计未来可再生航空燃料需求将增长。减少温室气体排放的一种可能性是在制备航空燃料时增加使用可再生燃料。源自诸如植物、树木、藻类、废物和其它有机物生物油等生物质的可再生喷气燃料为减少这些排放提供了机会。
各种标准中严格规定了不同类型的航空燃料。飞机和发动机燃料系统部件和燃料控制单元依靠燃料润滑其运动部件。例如，通过加氢处理生产的航空煤油型燃料的润滑性受到DEF STAN 91-091标准的限制，最大磨痕直径为0.85mm，这是使用称为BOCLE(气缸上滚珠润滑性评估器)的ASTM D5001测试方法测量的。无论何时在最终燃料共混物中使用合成燃料组分，都需要测量润滑性。燃料润滑性很重要，尤其是在军事用途中。
WO 2010/046590A2公开了一种具体的催化加氢处理方法，包含混合加氢处理或加氢裂化的石油衍生原料和加氢处理或加氢裂化的生物衍生原料，然后分馏。该方法可生产根据ASTM D5001，BOCLE润滑性为0.58mm的煤油。适用于该方法的生物衍生原料包含植物和/或动物脂肪或由植物和/或动物脂肪形成，其中相对于甘油三酯总重量，按重量计至少5％的脂肪酸具有小于或等于14个碳原子的链长。
WO 2019/129928A1公开了一种方法，包含裂解生物基材料，例如妥尔油沥青(TOP)，然后分馏以获得煤油。将该煤油与可再生喷气燃料混合。所得燃料共混物的BOCLE润滑性(ASTM D5001)为约0.75mm。
然而，仍然需要从包含可再生材料的原料生产航空燃料组分的稳健方法。
发明内容
下面给出一个简化的概述，以便提供对本发明各种实施方式的一些方面的基本理解。该概述不是本发明的广泛概述。其既不旨在识别本发明的主要或关键要素，也不旨在描绘本发明的范围。以下概述仅以简化形式呈现本发明的一些构思，作为对本发明的示例性实施方式的更详细描述的前奏。
据观察，当使包含化石加氢处理进料以及含有脂肪酸和松香的酯、游离脂肪酸和树脂酸的进料的混合物经受顺序加氢处理和加氢裂化反应条件时，可以获得满足航空燃料的ASTM D5001要求的BOCLE润滑性的航空燃料组分。
根据本发明，提供了一种生产航空燃料组分的新方法，该方法包含以下步骤：
a)提供包含按重量计75-95％的化石加氢处理进料和按重量计5-25％的第二进料的原料，该第二进料包含脂肪酸和松香的酯、游离脂肪酸和树脂酸，
b)使原料经受加氢处理反应条件以产生经加氢处理的流，
c)将至少部分的经加氢处理的流分离成
ο在大气压下沸点低于180℃的馏分，
ο在大气压下沸点在180℃和360℃之间的馏分，和
ο在大气压下沸点高于360℃的馏分，
d)使至少部分的在大气压下沸点高于360℃的馏分经受加氢裂化反应条件以产生经加氢裂化的流，
e)将至少部分的经加氢裂化的流与至少部分的经加氢处理的流混合以提供分馏流(fractionation stream)，
f)将分馏流至少分离成
ο在大气压下沸点低于180℃的馏分，
ο在大气压下沸点在180℃和360℃之间的馏分，和
ο在大气压下沸点高于360℃的馏分，和
g)从在大气压下沸点在180℃和360℃之间的一种或多种馏分中分离出航空燃料组分。
在所附从属权利要求中描述了本发明的多个示例性且非限制性的实施方式。
当结合附图阅读时，从具体示例性实施方式的以下描述，可以最佳地理解本发明和操作方法的各种示例性且非限制性的实施方式及其附加目的和优点。
动词“包含”和“包括”在本文件中用作开放限制，既不排除也不要求存在未列举的特征。除非另有明确说明，从属权利要求中列举的特征可以相互自由组合。此外，应当理解，在整个本文件中使用“一个”或“一种”，即单数形式，不排除复数。
附图说明
下面参考附图1更详细地解释本发明的示例性且非限制性实施方式及其优点，该图显示了用于将包含化石加氢处理进料和第二进料的原料加工成航空燃料组分的示例性系统，所述第二进料包含脂肪酸和松香的酯、游离脂肪酸和树脂酸。
具体实施方式
定义
如本文所定义的减压瓦斯油(VGO)是石油蒸馏留下的可在催化裂化单元中进一步精炼的重油。
如本文所定义的，化石加氢处理进料是一种包含化石VGO和在大气压下沸点低于360℃的化石瓦斯油组分的组合物。示例性化石加氢处理进料包含石脑油、轻质瓦斯油、瓦斯油、轻质减压瓦斯油、重质减压瓦斯油和重质瓦斯油。
如本文所定义的，妥尔油沥青(TOP)是来自妥尔油蒸馏的残余物。其主要含有脂肪酸和松香的高沸点酯、游离脂肪酸、树脂酸和不皂化物。妥尔油沥青可被视为REACH定义下的UVCB物质(未知或可变组成的物质，复杂反应产物或生物材料)。根据Holmbom(1978)的TOP组成如表1所示。妥尔油沥青通常包含占妥尔油沥青总重量的34至51wt％的游离酸、23至37wt％的酯化酸和25至34wt％的不皂化中性化合物。游离酸通常选自由脱氢枞酸、枞酸和其它树脂酸的组。酯化酸通常选自由油酸和亚油酸组成的组。不皂化物中性化合物通常选自由二萜甾醇、脂肪醇、甾醇和脱水甾醇组成的组。
表1.妥尔油沥青的组分组组成(沥青的wt％)a
Figure BDA0003666772220000051
a)Holmbom B.,
Figure BDA0003666772220000052
V.1978.Composition of Tall oil pitch,Journal of theAmerican oil chemistry society,55 342-344.
如本文所定义，在大气压下沸点低于180℃的馏分含有超过90wt.-％的沸点低于180℃(在常压下，即约1巴绝对压力下)的组分，在大气压下沸点在180℃和360℃之间的馏分含有超过90wt.-％的沸点在180℃和360℃之间(在常压下，即约1巴绝对压力)的组分，以及在大气压下沸点高于360℃的馏分含有超过90wt.-％的沸点高于360℃(在常压下，即约1巴绝对压力)的组分。
如本文所定义，加氢处理是有机化合物在高压氢气存在下去除氧(脱氧)和其它杂原子(氮、硫和氯)的反应。
如本文所定义，加氢裂化是通过在高压下和在催化剂存在下添加氢气，将石油的烃分子分解成更简单的分子(例如汽油或煤油)的过程。
本发明方法的原理如图1所示。该方法包含以下步骤：
a)提供原料10，其包含按重量计75-95％的化石加氢处理进料和按重量计5-25％的包含脂肪酸和松香的酯、游离脂肪酸和树脂酸的第二进料，
b)在反应器(A)中使原料经受加氢处理反应条件以产生经加氢处理的流20，
c)将至少部分的经加氢处理的流分离成
ο在大气压下沸点低于180℃的馏分30，
ο在大气压下沸点在180℃和360℃之间的馏分40，和
ο在大气压下沸点高于360℃的馏分50，
d)使至少部分的在大气压下沸点高于360℃的馏分在反应器(D)中经受加氢裂化反应条件以产生经加氢裂化的流60，
e)将至少部分的经加氢裂化的流与至少部分的经加氢处理的流混合，以提供分馏流70，
f)将分馏流至少分离成
ο在大气压下沸点低于180℃的馏分，
ο在大气压下沸点在180℃和360℃之间的馏分，
ο在大气压下沸点高于360℃的馏分，和
g)从在大气压下沸点在180℃和360℃之间的一种或多种馏分中分离出航空燃料组分80。
化石加氢处理进料通常包含石脑油、轻质瓦斯油、瓦斯油、一种或多种轻质减压瓦斯油馏分、重质减压瓦斯油。根据一个示例性实施方式，化石加氢处理进料包含石脑油、轻质瓦斯油、瓦斯油、一种或多种轻质减压瓦斯油馏分、重质减压瓦斯油和重质瓦斯油。
根据一个实施方式，第二进料包含按重量计50-100％的妥尔油沥青，优选按重量计75-100％的妥尔油沥青，更优选按重量计90-100％的妥尔油沥青，甚至更优选按重量计100％的妥尔油沥青。示例性的第二进料是妥尔油沥青。
示例性化石加氢处理进料包含按重量计6-32％的石脑油、按重量计8-32％的轻质瓦斯油、按重量计2-23％的瓦斯油、按重量计10-47％的一种或多种轻质减压瓦斯油馏分、按重量计8-51％的重质减压瓦斯油和按重量计0-40％的重质瓦斯油，因此组分之和为100％。
示例性原料包含按重量计80％的化石加氢处理进料和按重量计20％的包含脂肪酸和松香的酯、游离脂肪酸和树脂酸的第二进料。另一种示例性原料包含按重量计80％的化石加氢裂化进料和按重量计20％的妥尔油沥青。
根据示例性的非限制性实施方式，所述方法在两个顺序反应器(A,D)和两个蒸馏单元(B,C)中进行。该方法的步骤b)通常在第一反应器(A)中在温和加氢裂化工艺条件(MHC)下进行。步骤b)的主要目的是去除进料中的氮、硫和酸度。加氢处理反应条件通常包含LHSV 0.5-2.0h-1，优选0.7-1.2h-1，压力100-200巴表压(barg)，优选130-160巴表压，操作温度350-450℃，优选370-430℃，H2/进料400-1000dm3/dm3，和一种或多种加氢处理催化剂。步骤b)的示例性的非限制性反应条件包含LSHV 0.8h-1，压力147巴表压，温度380℃和H2/进料950dm3/dm3。该反应在本领域已知的一种或多种加氢处理催化剂的存在下进行。
分离步骤c)通常包含使用两个蒸馏单元(B,C)的蒸馏。第一蒸馏单元(B)通常用于将在大气压下沸点低于180℃的馏分30从经加氢处理的流20和经加氢裂化的流60中分离出来。馏分30主要包含汽油。将沸点高于180℃的剩余馏分进料到第二蒸馏单元(C)，其中将在大气压下沸点在180℃和360℃之间的馏分40与在大气压下沸点高于360℃的馏分50相分离。在大气压下沸点在180℃和360℃之间的馏分包含航空燃料组分80(即“煤油馏分”)并且通常还包含柴油90。
在进行加氢裂化之前，优选将部分馏分50作为排出物(bleed)100从系统中去除(remove，取出)。排出物的优选量为馏分50的按重量计至少10％，通常为馏分50的按重量计10-20％。去除的目的是避免流中最重的组分聚集到方法中使用的系统中且特别是第二反应器中。此外，去除用于获得所需的转化水平。
步骤d)包含将至少部分馏分50进料到反应器(D)中进行加氢裂化以产生经加氢裂化的流60。步骤d)的目的是使经加氢处理的流进一步裂化，并获得所需的转化水平。步骤d)的加氢裂化反应条件通常包含LHSV 0.5-2.0h-1，优选0.8-1.5h-1，压力100-200巴表压，优选130-160巴表压，操作温度330-390℃，优选340-380℃，H2/进料400-1000dm3/dm3，以及一种或多种加氢裂化催化剂。催化剂可以是本领域已知的任何HDO催化剂。示例性HDO催化剂选自由NiMo-、CoMo-、NiW-催化剂及其任何混合物组成的组。优选地，HDO催化剂是硫化的NiW、NiMo或CoMo催化剂。
步骤d)的示例性反应条件是LSHV 1h-1、压力147巴表压、温度340℃且H2/油进料850dm3/dm3。该反应在本领域已知的一种或多种加氢裂化催化剂存在下进行。
在步骤e)中，将至少部分经加氢裂化的流60与至少部分经加氢处理的流20混合，以产生分馏流70。
在步骤f)中，分馏流被分离成在大气压下沸点低于180℃的馏分、在大气压下沸点在180℃和360℃之间的馏分和在大气压下沸腾高于360℃的馏分。将至少部分在大气压下沸点高于360℃的馏分再循环回加氢裂化步骤。在进行加氢裂化之前，优选将部分馏分50作为排出物100从系统中去除。排出物的优选量为馏分50的按重量计至少10％，通常为馏分50的按重量计10-20％。该过程可以持续进行，直到所有原料都被消耗掉或收到所需的转化水平。
当该过程开始时，从第一反应器(A)进料到蒸馏单元(B,C)的流通常由经加氢处理的流20组成。当该过程进行时，经加氢裂化的流60与经加氢处理的流20混合，并形成分馏流70。当所有原料已被消耗时，经加氢裂化的流的摩尔分数可能上升到1。然而，可以通过调节系统中的流量来调节流20和60的比率。
在步骤f)中，将航空燃料组分80与在大气压下沸点在180℃和360℃之间的一种或多种馏分40相分离。分离可以在蒸馏单元如(B)中进行。根据一个优选的实施方式，分离在非原位薄膜蒸馏塔(E)中进行，以获得沸点在180-240℃之间的馏分，即航空燃料组分80，并且优选还获得沸点在240-360℃之间的馏分，即柴油90。
实验性的
该过程中使用的示例性进料组分列于表2。该进料含有按重量计80％的化石加氢处理进料和按重量计20％的妥尔油沥青。工艺条件列于表3。
表2.实验中使用的原料。
共混组分 裂化的化合物+TOP(kg) 裂化的化合物+TOP(％)
石脑油 26 11.1
轻质瓦斯油 38 16.2
瓦斯油 10 4.3
轻质VGO，较轻的馏分 33 14.1
轻质VGO，较重的馏分 27 11.5
重质减压瓦斯油 33 14.1
重质瓦斯油 20 8.5
TOP 47 20.1
总计 234 100.0
表3.工艺条件
条件 加氢处理 加氢裂化
<![CDATA[LHSV(h<sup>-1</sup>)]]> 0.8 1
压力(巴) 147 147
温度SOR(℃) 380 345
<![CDATA[H<sub>2</sub>/油进料(dm<sup>3</sup>/dm<sup>3</sup>)]]> 950 850
该过程使用两个顺序反应器(A,D)和两个蒸馏单元(B,C)运行。MHC中第一反应器的目的是去除进料中的氮、硫和酸度。第二反应器的目的是进一步裂化进料并且调整转化率以获得所需的排出水平。调整蒸馏单元以将产物分离为沸点低于180℃的馏分、沸点在180℃和360℃之间的馏分和沸点高于360℃的馏分。在非原位薄膜蒸馏塔中进行180-360℃馏分的进一步分离，以获得180-240℃(航空燃料组分)和240-360℃(柴油)产品馏分。对分离的煤油馏分进行分析。结果列于表4。
如从表3看出的，航空燃料组分的BOCLE润滑性低于航空燃料规范DEF STAN 91-091的0.85mm的最大水平。因此，本发明可用于在没有润滑改进剂添加剂的情况下改进燃料润滑性或改进润滑不良的燃料组分。
表4.蒸馏的航空燃料组分的分析结果。
Figure BDA0003666772220000101
Figure BDA0003666772220000111
a)蒸馏-05、蒸馏-10等＝在1atm下在限定温度下沸腾的馏分的％。
以上给出的描述中提供的具体示例不应被解释为限制所附权利要求的范围和/或适用性。

Claims (19)

1.一种用于生产航空燃料组分的方法，所述方法包括
a)提供包含按重量计75-95％的化石加氢处理进料和按重量计5-25％的第二进料的原料，所述第二进料包含脂肪酸和松香的酯、游离脂肪酸和树脂酸，
b)使所述原料经受加氢处理反应条件以产生经加氢处理的流，
c)将至少部分的所述经加氢处理的流分离成
○在大气压下沸点低于180℃的馏分，
○在大气压下沸点在180℃和360℃之间的馏分，和
○在大气压下沸点高于360℃的馏分，
d)使至少部分的所述在大气压下沸点高于360℃的馏分经受加氢裂化反应条件以产生经加氢裂化的流，
e)将至少部分的所述经加氢裂化的流与至少部分的所述经加氢处理的流混合，以提供分馏流，
f)将所述分馏流至少分离成
○在大气压下沸点低于180℃的馏分，
○在大气压下沸点在180℃和360℃之间的馏分，
○在大气压下沸点高于360℃的馏分，以及
g)从在大气压下沸点在180℃和360℃之间的一种或多种馏分中分离出航空燃料组分。
2.根据权利要求1所述的方法，其中，所述第二进料包含按重量计50-100％的妥尔油沥青。
3.根据权利要求1或2所述的方法，其中，步骤d)包括：在所述经受之前，去除按重量计至少10％的所述在大气压下沸点高于360℃的馏分。
4.根据权利要求1或2所述的方法，包括将步骤f)的至少部分的所述在大气压下沸点高于360℃的馏分再循环至步骤d)。
5.根据权利要求1或2所述的方法，其中，所述化石加氢处理进料包含石脑油、瓦斯油。
6.根据权利要求1或2所述的方法，其中，所述原料包含按重量计80％的化石加氢处理进料和按重量计20％的妥尔油沥青。
7.根据权利要求1或2所述的方法，其中，步骤b)的所述加氢处理反应条件包括：LHSV0.5-2.0h-1；压力100-200巴表压；操作温度350-450℃；H2/进料400-1000dm3/dm3；以及一种或多种加氢处理催化剂。
8.根据权利要求1或2所述的方法，其中，步骤d)的所述加氢裂化反应条件包括：LHSV0.5-2.0h-1；压力100-200巴表压；操作温度330-390℃；H2/进料400-1000dm3/dm3；以及一种或多种加氢裂化催化剂。
9.根据权利要求1或2所述的方法，其中，所述分离包括蒸馏。
10.根据权利要求1或2所述的方法，包括将步骤g)的所述在大气压下沸点在180℃和360℃之间的一种或多种馏分分馏成
○在大气压下沸点在180-240℃的馏分，和
○在大气压下沸点在240-360℃的馏分。
11.根据权利要求10所述的方法，其中，所述分馏包括薄膜蒸馏。
12.根据权利要求1所述的方法，其中，所述第二进料包含按重量计75-100％的妥尔油沥青。
13.根据权利要求1所述的方法，其中，所述第二进料包含按重量计90-100％的妥尔油沥青。
14.根据权利要求1所述的方法，其中，所述第二进料包含按重量计100％的妥尔油沥青。
15.根据权利要求1或2所述的方法，其中，步骤d)包括：在所述经受之前，去除按重量计10-20％的所述在大气压下沸点高于360℃的馏分。
16.根据权利要求1或2所述的方法，其中，所述化石加氢处理进料包含轻质瓦斯油。
17.根据权利要求1或2所述的方法，其中，所述化石加氢处理进料包含轻质减压瓦斯油、重质减压瓦斯油。
18.根据权利要求1或2所述的方法，其中，步骤b)的所述加氢处理反应条件包括：LHSV0.7-1.2h-1；压力130-160巴表压；操作温度370-430℃；H2/进料400-1000dm3/dm3；以及一种或多种加氢处理催化剂。
19.根据权利要求1或2所述的方法，其中，步骤d)的所述加氢裂化反应条件包括：LHSV0.8-1.5h-1；压力130-160巴表压；操作温度340-380℃；H2/进料400-1000dm3/dm3；以及一种或多种加氢裂化催化剂。
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