CN101942336A - 一种生产低浊点高粘度指数润滑油基础油的方法 - Google Patents
一种生产低浊点高粘度指数润滑油基础油的方法 Download PDFInfo
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- CN101942336A CN101942336A CN201010274479XA CN201010274479A CN101942336A CN 101942336 A CN101942336 A CN 101942336A CN 201010274479X A CN201010274479X A CN 201010274479XA CN 201010274479 A CN201010274479 A CN 201010274479A CN 101942336 A CN101942336 A CN 101942336A
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- isomerization
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- 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
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/304—Pour point, cloud point, cold flow properties
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4018—Spatial velocity, e.g. LHSV, WHSV
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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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/02—Gasoline
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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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/10—Lubricating oil
Abstract
本发明涉及一种生产低浊点高粘度指数润滑油基础油的方法;采用初馏点为300℃~460℃的含蜡量为≥5%、倾点≥-20℃、浊点为≥-5℃的高含蜡重质馏份油为原料,在氢气存在的情况下,通过加氢预精制-异构化/非对称裂化-补充精制反应过程生产低倾点和低浊点高粘度指数润滑油基础油,联产优质石脑油、中间馏分油的生产方法;主要特点是重质基础油收率高且倾点和浊点低,基础油粘度大和粘度指数高。
Description
技术领域:
本发明涉及一种生产低浊点(<-5℃)高粘度指数(>120)润滑油基础油的方法。
背景技术:
专利CN101134910A提供一种降低润滑油馏分油倾点、浊点的方法。该方法采用催化脱蜡工艺,催化剂为一种由包括在一种含ZSM-5分子筛的载体中以镍金属作为活性组分,可以将倾点为9℃的轻脱沥青加氢处理油降低到-24℃,浊点从12℃降低到-16℃。该方法明显的缺点是当原料油中蜡含量高、降倾点和浊点幅度需要加大时,基础油产品收率和粘度会大幅度降低。
专利CN 1524929提供一种降低润滑油基础油浊点的方法,润滑油料先经溶剂预脱蜡后脱蜡油的倾点为-5℃~15℃;预脱蜡油经加氢处理降低其硫、氮含量;加氢处理后的预脱蜡油经异构脱蜡可以得到较低浊点的润滑油基础油。为避免增加反应的苛刻度而造成裂化反应加剧,该方法需要首先用预先溶剂脱蜡过程将大部分蜡脱除,然后经过加氢处理和异构脱蜡过程。该方法提出脱蜡油的倾点不应高于15℃,否则异构化产物的浊点难以达到0℃以下,甚至难以达到5℃以下。
美国专利US 6,699,385公开了一种通过异构脱蜡过程降低浊点的方法,为避免增加反应的苛刻度而造成裂化反应加剧,需要先将含蜡原料油进行分馏,用较轻的馏分进行异构脱蜡,且浊点仅能降低到0℃左右。
上述已公开专利和文献所阐述的润滑油基础油脱蜡的方法都没有阐明或隐含通过异构化-非对称裂化反应过程生产具有低倾点和低浊点、高粘度指数等特性基础油的方法,而且与公开专利和文献所阐述的方法相比,异构化-对称裂化反应过程的基础油收率尤其是重质基础油收率更高。
发明内容
本发明的目的是提供一种生产低浊点(<-5℃)高粘度指数(>120)润滑油基础油的方法,采用初馏点为300℃~460℃的含蜡量为≥5%、倾点≥-20℃、浊点为≥-5℃的高含蜡重质馏份油为原料,通过加氢预精制-异构化/非对称裂化-补充精制三段加氢反应过程,生产低倾点高粘度指数API(美国石油学会)II、III(分类标准见表1)类润滑油基础油的方法,异构化/非对称裂化反应包含异构化和非对称裂化两种化学反应。在发生异构化反应的同时,原料油中的高倾点直链烷烃和高倾点大分子少支链异构烷烃发生非对称裂化反应。所谓非对称裂化反应是指加氢裂化反应发生在临近链烷烃分子两端的某个C-C键上,生成一大一小两个较小的分子,其中的小分子属于气体和石脑油馏分,大分子则属于润滑油基础油馏分。
非对称裂化反应是通过选用具有特殊孔道结构的10元环复合分子筛作催化剂载体,以增强催化剂孔道对正构烷烃和少支链异构烷烃的内扩散限制,使裂化反应优先选择在临近正构烷烃两端的位置发生,可以大幅提高基础油产品、尤其是重质基础油产品的收率。
异构化/非对称裂化反应的特征在于产品呈双峰分布,即轻组分(气体和石脑油)和低倾点、低浊点重质基础油收率高,中间馏份油(煤油和柴油)收率低。该方法可以解决采用重质高含蜡油生产润滑油基础油时,通过溶剂精制、溶剂脱蜡等物理方法和/或加氢处理、催化脱蜡、加氢处理、加氢裂化等化学方法生产润滑油基础油时目的产品收率低、倾点和浊点高、芳烃含量高、粘度指数低等问题。
本发明提供的生产方法包括:(1)加氢预精制反应过程,在一定的氢气压力下,含蜡原料油与加氢预精制催化剂接触,发生脱硫、脱氮、芳烃饱和及开环反应。加氢预精制反应的产物由汽提塔分离,塔底馏分进入加氢异构化/非对称裂化反应过程;(2)加氢异构化/非对称裂化反应过程,在一定的氢气压力下,汽提塔塔低产物与异构化-非对称裂化催化剂接触,发生异构化-非对称裂化和加氢饱和反应,得到低倾点、低浊点、低芳烃高粘度指数产物,全部产物直接进入加氢补充精制反应过程;(3)加氢补充精制反应过程,在一定的氢气压力下,异构化-非对称裂化反应产物与加氢补充精制催化剂接触,进一步发生加氢饱和反应,得到光安定性和热稳定性好的补充精制油品;(4)产品分离过程,加氢补充精制反应过程得到的产物经过热高压分离器和冷低压分离器将气液两相产物分离,液体产物再经过常压分馏塔和减压分馏塔采出石脑油、煤油、柴油和低倾点、高粘度指数的轻、中、重质润滑油基础油。
按照本发明提供的方法,所述的原料油包括糠醛精制油、蜡下油、蜡膏(软蜡)、丙烷脱沥青油、加氢裂化尾油、费-托合成蜡、减压瓦斯油含蜡油中的一种或几种油品的混合物。
按照本发明提供的方法,所述的加氢预精制催化剂含有60重量%~90重量%的氧化铝、氧化硅、氧化钛中的一种或几种复合氧化物,和10重量%~40重量%的三氧化钼、三氧化钨、氧化镍、氧化钴中的一种或几种复合氧化物。
按照本发明提供的方法,所述的加氢预精制催化剂在使用前,通常在氢气存在条件下,在150~350℃温度用硫化氢或含硫原料油进行预硫化。这种预硫化反应可以在器外进行也可以在器内原位硫化。
按照本发明提供的方法,所述的加氢预精制反应的工艺条件为:反应温度为350℃~410℃,氢分压为10MPa~18MPa,空速(LHSV)为0.5h-1~2.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3。
按照本发明提供的方法,所述的加氢预精制产品经气提分离后得到油品的总硫含量≯10μg/g,总氮含量≯5μg/g。
按照本发明提供的方法,异构化-非对称裂化催化剂的特征在于采用下述一维10元环中孔复合分子筛中的至少一种:ZSM-22/ZSM-23复合分子筛、ZSM-23/ZSM-22复合分子筛、ZSM-5/SAPO-11复合分子筛、ZSM-22/SAPO-11复合分子筛、ZSM-23/SAPO-11复合分子筛、EU-1/SAPO-11复合分子筛、N U-87/SAPO-11复合分子筛。分子筛含量为40%~80%,其余为氧化铝和至少一种VIII族贵金属为Pt和/或Pd,贵金属含量为0.3重量%~0.6重量%。催化剂平均孔径为0.3nm~0.8nm,平均孔体积为0.1ml/g~0.4ml/g,BET比表面积为120m2/g~300m2/g。
按照本发明提供的方法,所述的异构化/非对称裂化催化剂在使用前,需要在氢气存在的条件下,在150~450℃温度下进行预还原。
按照本发明提供的方法,所述的异构化/非对称裂化反应的工艺条件为:反应温度为260℃~410℃,氢分压为10MPa~18MPa,体积空速为0.5h-1~3.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3。
按照本发明提供的方法,所述的加氢补充精制催化剂由一种无定形硅铝和至少一种VIII族贵金属组成。
按照本发明提供的方法,加氢补充精制催化剂的特征在于,SiO2∶Al2O3为1∶1~1∶9,平均孔半径为1.0nm~5.0nm,孔体积为0.3ml/g~1.0ml/g,BET比表面积为260m2/g~450m2/g。所述的贵金属为Pt和/或Pd,其含量为0.3重量%~0.6重量%。
按照本发明提供的方法,所述的加氢补充精制催化剂在使用前,通常在氢气存在条件下,于150~450℃温度下进行预还原。
按照本发明提供的方法,所述的加氢补充精制反应条件为:反应温度为180℃~320℃,氢分压为10MPa~18MPa,体积空速为0.5h-1~3.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3。
按照本发明提供的方法,所述的常、减压蒸馏过程是将补充精制后的油品混合物经过常、减压蒸馏分离,最后得到石脑油、中间馏份油和润滑油基础油。
本发明采用初馏点为300℃~460℃的含蜡量为≮5%、倾点≮-20℃、浊点为≮-5℃的高含蜡重质馏份油为原料,通过加氢预精制-异构化/非对称裂化-补充精制三段加氢反应过程,生产低倾点高粘度指数API(美国石油学会)II、III(分类标准见表1)类润滑油基础油的方法。具体涉及加氢异构化-非对称裂化这一关键反应过程。该方法的特点是对重质高含蜡原料油的适应性好、重质基础油产品收率高、产品粘度、粘度指数、倾点和浊点等技术指标好,同时可联产优质石脑油和少量中间馏分油。
表1API润滑油基础油分类标准
附图说明
图1实施例1与对比例1产品分布情况
图2实施例2与对比例2产品分布情况
图3润滑油基础油异构化-非对称裂化/补充精制生产工艺流程图
图4润滑油基础油预处理/异构脱蜡/补充精制生产工艺流程图
图5润滑油基础油预精制/异构化-非对称裂化/补充精制生产工艺流程图
图6润滑油基础油异构化-非对称裂化/补充精制生产工艺流程图
具体实施方式
下面的实施例将对本发明做进一步说明。
本发明各个实施例中所使用的加氢预精制催化剂和补充精制催化剂及其制备方法简述如下:
本发明中各实施例和对比例中采用相同的加氢预精制催化剂和加氢补充精制催化剂。加氢预精制催化剂按照下述方法制备:选取具有适当孔结构的拟薄水铝石制备成横截面为三叶草形状的条状载体,干燥和焙烧后,用浸渍法将Ni元素和Mo元素负载在氧化铝载体上,经烘干、焙烧制备成加氢预精制催化剂,得到的催化剂NiO含量为4.20%,MoO3的含量为18.3%,其余为氧化铝,催化剂比表面积为175m2/g,孔体积为0.45cm3/g。
各实施例中所采用的异构化/非对称裂化催化剂均按照专利CN1762594A中实施例12中所述的方法制备成0.5%Pt/ZSM-22/SAPO-11催化剂。
加氢补充精制催化剂的制备方法:载体采用的无定形硅铝通过使用并流固定pH值、硅铝共沉淀的方法制备。载体烘干、焙烧后,挤压成横截面为三叶草的条状,烘干焙烧后用浸渍法负载金属Pt,再经过干燥和焙烧制备成加氢补充精制催化剂,得到的催化剂Pt含量为0.51%,其余为氧化硅和氧化铝,SiO2∶Al2O3为1∶6.3,比表面积为305cm2/g,孔体积为1.08cm3/g。
对比例1
采用US4440871实施例18中所述的方法合成SAPO-11分子筛,取SAPO-11分子筛原粉,按照70%SAPO-11分子筛和30%拟薄水铝石的比例,加上少量HNO3水溶液等黏合剂混捏成φ1.2mm的条状,在110℃烘干24小时,600℃焙烧24小时,粉碎至长度为1mm-2mm的颗粒。取足量的载体颗粒,采用通常的充填孔浸渍方法将适量的浓度为3%的Pt(NH3)4Cl2溶液浸渍16小时,然后在120℃烘干4小时,480℃焙烧8小时。取所制备的催化剂200ml,在催化剂装填量为200ml的高压加氢反应试验装置上用纯氢原位预还原,得到0.5%Pt/SAPO-11催化剂。异构脱蜡催化剂还原条件:氢气流速2000mL/h,以5℃/min升至250℃恒温2小时。再以5℃/min升至450℃,恒温2小时后,在氢气流中调整至反应温度。采用图4所示的加氢预精制-异构脱蜡-加氢补充精制工艺方法和表3所列的工艺条件,以石蜡基650N糠醛精制油作原料,其物化性质见表2。加氢预精制和补充精制催化剂与上述实施例所述催化剂相同。
实施例1
按照图4所示的工艺方法,试验装置和原料油与对比例1相同。除了异构化/非对称裂化的反应温度为351℃、空速为0.75h-1外,其他反应条件与对比例1相同,对比例1的反应条件详见表3。
实施例1和对比例1产品分布对比情况见表4,主要产品性质见表5。
按照图4所示的工艺方法,在对比例1所述的试验装置上,用石蜡基200SN浅度脱蜡油作原料油,其物化性质见表2,反应条件见表3。
表2对比例1和实施例1的原料油性质
表3对比例1和实施例1采用的反应条件
表4对比例1和实施例1的产品分布
表5对比例1和实施例1的重质基础油产品性质
分析项目 | 对比例1 | 实施例1 | 分析方法 |
初馏点,℃ | 421 | 385 | GB/T 9168 |
20℃密度,g/cm3 | 0.8424 | 0.8524 | GB/T 1884 |
倾点,℃ | -15 | -15 | GB/T 3535 |
浊点,℃ | 5 | -6 | GB/T6986-86 |
芳烃含量,% | 1.2 | 0 | |
开口闪点,℃ | 265 | 270 | GB/T3536 |
比色,号 | +30 | +30 | GB/T3555 |
40℃运动粘度,mm2/s | 60.89 | 61.06 | GB/T265 |
100℃运动粘度,mm2/s | 9.313 | 9.423 | GB/T265 |
粘度指数 | 132 | 136 | GB/T 1995 |
从表2~5以及图1可以看出,实施例1所述的加氢预精制、异构化-非对称裂化、补充精制反应过程中采用的原料油倾点高达60℃,说明该原料油含有大量高碳数蜡分子。实施例1和对比例1所述的方法中,在发生异构化反应的同时也会发生加氢裂化反应,但与对比例1所述的传统加氢裂化反应不同,实施例1表现出明显的非对称裂化反应的特点,即C-C键的断裂优先选择在临近长链烷烃两端的位置发生,使小分子产物(气体和石脑油)和大分子产物(10cst基础油)的收率都较高,分别达到19.96%和73.3%,而柴油和轻质基础油(2cst基础油)收率分别只有2.96%和3.78%。对比例1所述的方法所发生的裂化反应则选择在临近长链烷烃的中间位置进行,小分子产物(气体+石脑油)和大分子产物(10cst基础油)的收率分别为15.71%和47.85%,都比实施例1低,柴油和轻质基础油(2cst基础油)的收率分别为11.58%和24.86%,比实施例1高。同时,实施例1的重质基础油产品浊点比对比例1低11℃。实施例1的重质基础油产品粘度指数比对比例1高4个单位。
对比例2
采用US5783168实施例2中所述的方法合成ZSM-22分子筛,取适量ZSM-23分子筛原粉,按照70%ZSM-22分子筛和30%拟薄水铝石的比例,加上少量HNO3水溶液等黏合剂混捏成φ1.2mm的条状,在110℃烘干24小时,600℃焙烧24小时,粉碎至长度为1mm-2mm的颗粒。取足量的载体颗粒,采用通常的充填孔浸渍方法将适量的浓度为3%的Pt(NH3)4Cl2溶液浸渍16小时,然后在120℃烘干4小时,480℃焙烧8小时。取所制备的催化剂200ml,在催化剂装填量为200ml的高压加氢反应试验装置上用纯氢原位预还原,得到0.5%Pt/ZSM-22。催化剂还原条件与对比例1相同。以石蜡基200SN脱蜡油作原料,其物化性质见表6,采用加氢预精制-异构脱蜡-加氢补充精制串联工艺方法(图4所示)和表7所列的工艺条件,
实施例2
工艺方法、试验装置和原料油与对比例2相同。除了异构化/非对称裂化反应温度为325℃、空速为1.2h-1外,其他反应条件与对比例2相同。
实施例2和对比例2反应过程的产品分布见表8,主要产品性质见表9。
从表6~9以及图2可以看出,与对比例2相比,实施例2所述的方法具有明显的加氢预精制-异构化/非对称裂化-补充精制反应过程的特征,即重质基础油(5cst基础油)收率高,且得到的小分子产物(气体和石脑油)和大分子产物(10cst基础油)的收率都较高,分别达到19.96%和73.3%,柴油和轻质基础油(2cst基础油)收率分别只有2.96%和3.78%。产品分布呈双峰分布。同时可以看出,实施例2的重质基础油产品浊点对比例2低10℃。
表6原料油性质
表7对比例1、2的反应条件
表8实施例1、2和对比例1、2产品分布
表9对比例2和实施例2的重质基础油产品性质
分析项目 | 对比例2 | 实施例2 | 分析方法 |
初馏点,℃ | 400 | 394 | GB/T9168 |
20℃密度,g/cm3 | 0.8521 | 0.8629 | GB/T1884 |
倾点,℃ | -18 | -21 | GB/T3535 |
浊点,℃ | -5 | -15 | GB/T6986-86 |
开口闪点,℃ | 220 | 235 | GB/T3536 |
比色,号 | +30 | +30 | GB/T3555 |
40℃运动粘度,mm2/s | 34.56 | 39.39 | GB/T265 |
100℃运动粘度,mm2/s | 5.713 | 6.273 | GB/T 265 |
粘度指数 | 104 | 105 | GB/T1995 |
实施例3
按照图4所示的工艺方法,试验装置与对比例1相同,原料油是原油经过减压蒸馏、糠醛精制和酮苯脱蜡等工序得到的100N蜡膏,其物化性质在表10中列出。在表11所列的工艺条件下,得到的产品分布见表12,主要产品性质见表13。
实施例4
按照图4所示的工艺方法,试验装置与对比例1相同,原料油为表10中列出的400N蜡膏。在表11所列的工艺条件下,产品分布情况见表12,主要产品性质见表13。
从表10~13可以看出,实施例3的异构化/非对称裂化反应产品分布与实施例1、2相似,产物以轻组分产物(气体和石脑油)和2cst基础油产物为主,两者收率分别为17.32%和70.83%,柴油收率为11.87%,呈现了轻组分和重组分产品收率高、中间馏分收率低的双峰分布。实施例4的产品分布与实施例3的相似,且双峰分布的特征更加明显。实施例3、4的2cst和6cst基础油产品的倾点和浊点都很低,6cst基础油的粘度指数达到123,满足API III类基础油的要求。
表10实施例3、4的原料油性质
分析项目 | 100N蜡膏 | 400N蜡膏 |
20℃密度,g/cm3 | 0.8319 | 0.8643 |
40℃粘度,mm2/s | 8.292 | 41.77 |
100℃粘度,mm2/s | 2.476 | 7.205 |
粘度指数 | 128 | 136 |
倾点,℃ | 27 | 33 |
硫含量,μg/g | 490 | 534 |
氮含量,μg/g | 176 | 430 |
化学族组成,% | ||
饱和烃 | 90.11 | 83.51 |
芳烃 | 9.17 | 15.35 |
极性化合物 | 0.72 | 1.14 |
馏程,℃HK | 307 | 370 |
5% | 342 | 422 |
10% | 348 | 450 |
30% | 358 | 469 |
50% | 367 | 477 |
70% | 376 | 486 |
90% | 386 | 498 |
95% | 392 | 505 |
KK | 404 | 510 |
表11实施例3、4的工艺条件
表12实施例3、4的产品分布
表13实施例3、4的基础油产品性质
实施例5
按照图4所示的工艺方法,试验装置与对比例1相同,原料油为表9中列出的650N蜡膏,是原油经过减压蒸馏、糠醛精制和酮苯脱蜡等工序得到的含蜡油品。在表14所列的工艺条件下,得到的产品分布见表15,主要产品性质见表16。
实施例6
按照图4所示的工艺方法,试验装置与对比例1相同,原料油为150BS蜡膏,是石蜡基原油经过减压蒸馏、丙烷脱沥青、糠醛精制和酮苯脱蜡等工序得到的含蜡油品,其物化性质见表14,在表15所列的工艺条件下,得到的产品分布见表16,主要产品性质见表17。
从表14~17中可以看出,650SN蜡膏和150BS蜡膏的馏分很重,倾点也很高。对于这两种重质原料油,为使基础油倾点达到不高于-15℃的要求,降倾点幅度需要达到78℃。加氢预精制-异构化/非对称裂化-补充精制反应过程生成的小分子产物(气体和石脑油)和大分子产物(8cst和20cst基础油)收率高、中间馏份油(柴油+2cst基础油)收率低的特征明显。重质低倾点产品的粘度指数极高,可达到140以上,且倾点和浊点都能降低到很低。
表14实施例5、6的原料油性质
表15实施例5、6的工艺条件
表16实施例5、6的产品分布
表17实施例5、6的重质基础油产品性质
实施例7
加氢裂化尾油是减压馏份油经过加氢预处理-加氢裂化反应后生成的重质馏份油,所含的硫、氮等杂质已经脱除,大部分芳烃发生加氢饱和开环,不需要进行预精制反应脱硫、氮,也不需要预处理反应提高粘度指数,可采用图6所示的异构化-非对称裂化/补充精制工艺。在试验装置上进行加氢评价,采用一种物化性质如表18所示的加氢裂化尾油作原料油,在表19所列的工艺条件下,得到的产品分布见表120,主要产品性质见表21。从表18~21可以看出,低硫、氮含量,高粘度指数、高倾点的加氢裂化尾油。经过工艺条件缓和的异构化-非对称裂化/补充精制反应后,产品分布呈现出小分子产物(气体和石脑油)和大分子产物(8cst和20cst基础油)收率高、中间馏份油(柴油+2cst基础油)收率低的特点,同时产品的浊点达到-15℃。
表18实施例7的原料油性质
表19实施例7的工艺条件
工艺条件 | 异构化-非对称裂化 | 补充精制 |
平均温度,℃ | 310 | 230 |
氢分压,MPa | 12.4 | 12.4 |
体积空速,h-1 | 1.0 | 1.7 |
氢油比,Nm3/Nm3 | 350 | 350 |
表20实施例7的产品分布
产品 | 产品收率,% |
燃料气+石脑油 | 15.9 |
柴油 | 4.66 |
2cst基础油 | 1.09 |
4cst基础油 | 78.35 |
总基础油收率 | 79.44 |
表21实施例7的4cst基础油产品性质
分析项目 | 4cst基础油 | 分析方法 |
20℃密度,g/cm3 | 0.8288 | GB/T 1884 |
倾点,℃ | -18 | GB/T 3535 |
浊点,℃ | -15 | GB/T 6986-86 |
开口闪点,℃ | 204 | GB/T 3536 |
比色,号 | +30 | GB/T 3555 |
40℃运动粘度,mm2/s | 17.58 | GB/T 265 |
100℃运动粘度,mm2/s | 3.974 | GB/T 265 |
粘度指数 | 124 | GB/T 1995 |
实施例8
F-T合成蜡是经过Co基催化剂合成的以高碳数长链正构烷烃为主的烃类产品。合成蜡主要由碳数为C8~C45的正构链烷烃组成,最大碳数分布在C18前后。切去<320℃组分后的FT合成蜡的最大碳数分布略向高碳数移动。图1为采用Co基催化剂合成的产物以及经常压蒸馏切去320℃-组分后的F-T合成蜡的碳数分布图。F-T合成蜡基本不含硫、氮等杂质和芳烃,不需要进行预精制反应脱硫、氮,也不需要预处理反应提高粘度指数,可直接采用如图6所示的异构化-非对称裂化/补充精制工艺。异构脱蜡试验装置与对比例1相同,以F-T合成蜡中320℃+组分作原料油,其物化性质见表18,在表19所列的工艺条件下,得到的产品分布情况见表20,主要产品性质见表21。从表18~21可以看出,经过异构化-非对称裂化/补充精制反应过程后得到的产品分布呈现双峰分布的特征,同时2cst基础油产品的浊点达到-6℃,粘度指数高达162。
表18实施例8的原料油性质
表18实施例8的工艺条件
工艺条件 | 异构化-非对称裂化 | 补充精制 |
平均温度,℃ | 360 | 230 |
氢分压,MPa | 12.4 | 12.4 |
体积空速,h-1 | 0.5 | 0.85 |
氢油比,Nm3/Nm3 | 750 | 750 |
表19实施例8的产品分布
产品 | 产品收率,% |
燃料气+石脑油 | 23.7 |
柴油 | 6.63 |
2cst基础油收率 | 69.67 |
表20实施例8的产品性质
产品 | 2cst基础油 | 分析方法 |
20℃密度,g/cm3 | 0.8416 | GB/T 1884 |
倾点,℃ | -15 | GB/T 3535 |
浊点,℃ | -6 | GB/T 6986-86 |
开口闪点,℃ | 179 | GB/T 3536 |
比色,号 | +30 | GB/T 3555 |
40℃运动粘度,mm2/s | 9.756 | GB/T 265 |
100℃运动粘度,mm2/s | 2.912 | GB/T 265 |
粘度指数 | 162 | GB/T 1995 |
Claims (3)
1.一种生产低浊点高粘度指数润滑油基础油的方法,浊点<-5℃,粘度指数>120,其特征在于:采用初馏点为300℃~460℃的含蜡量为≥5%、倾点≥-20℃、浊点为≥-5℃的高含蜡重质馏份油为原料,在氢气存在的情况下,通过加氢预精制-异构化/非对称裂化-补充精制反应过程生产润滑油基础油;
(1)在加氢预精制反应过程中,含蜡重质原料油与预精制催化剂接触,发生脱硫、脱氮、芳烃饱和及开环反应,氢预精制反应生成的轻质产物作为副产品经汽提塔分离出去,重质产物进入异构化-非对称裂化反应过程;
加氢预精制反应工艺条件为:反应温度为350℃~410℃,氢分压为10MPa~18MPa,空速为0.5h-1~2.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3;
预精制催化剂:含有60重量%~90重量%的氧化铝、氧化硅、氧化钛中的一种或几种复合氧化物,和10重量%~40重量%的三氧化钼、三氧化钨、氧化镍、氧化钴中的一种或几种复合氧化物;
(2)在加氢异构化-非对称裂化反应过程中,预精制反应生成的重质产物与异构化-非对称裂化催化剂接触,高倾点的含蜡组分发生异构化-非对称裂化反应,转化成为低倾点的同分异构体和非对称裂化产物,然后直接进入补充精制反应过程;
加氢异构化-非对称裂化反应工艺条件为:反应温度为260℃~410℃,氢分压为10MPa~18MPa,体积空速为0.5h-1~3.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3;
催化剂:中孔分子筛的含量为40%~80%,Pt和/或Pd,含量为0.3重量%~0.7重量%,其余为氧化铝;
(3)在加氢补充精制反应过程中,低倾点的异构化-非对称裂化反应产物与补充精制催化剂接触,残留的芳烃和非对称裂化反应产生的烯烃被加氢饱和,再经分馏塔分离,最终得到润滑油基础油和气态烃、石脑油和中间馏份油;
催化剂由无定形硅铝和至少一种VIII族贵金属组成,SiO2∶Al2O3重量为1∶1~9,平均孔半径为1.Onm~5.0nm,孔体积为0.3ml/g~1.0ml/g,BET比表面积为260m2/g~450m2/g;贵金属为Pt和/或Pd,其含量为0.3重量%~0.6重量%;
加氢补充精制反应条件为:反应温度为180℃~320℃,氢分压为10MPa~18MPa,体积空速为0.5h-1~3.0h-1,氢油体积比为300Nm3/m3~1000Nm3/m3。
2.根据权利要求1所述的生产低浊点高粘度指数润滑油基础油的方法,其特征在于:所述的重质原料油包括糠醛精制油、蜡下油、蜡膏、丙烷脱沥青油、加氢裂化尾油、减压瓦斯油、费-托合成蜡中的一种或几种油品的混合物。
3.根据权利要求1所述的生产低浊点高粘度指数润滑油基础油的方法,其特征在于:加氢异构化-非对称裂化反应催化剂所采用的中孔分子筛为ZSM-22/ZSM-23复合分子筛、ZSM-23/ZSM-22复合分子筛、ZSM-22/SAPO-11复合分子筛、ZSM-23/SAPO-11复合分子筛、ZSM-5/SAPO-11复合分子筛、EU-1/SAPO-11复合分子筛中的一种。
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CN104080891A (zh) * | 2012-05-09 | 2014-10-01 | 雪佛龙美国公司 | 用于制备高vi润滑油的方法 |
CN103627428A (zh) * | 2012-08-23 | 2014-03-12 | 中国石油化工股份有限公司 | 一种生产低凝点润滑油基础油的加氢方法 |
CN103627428B (zh) * | 2012-08-23 | 2015-11-25 | 中国石油化工股份有限公司 | 一种生产低凝点润滑油基础油的加氢方法 |
CN103289738B (zh) * | 2013-06-25 | 2015-10-28 | 中石化南京工程有限公司 | 一种加氢裂化尾油加氢生产高档润滑油基础油的组合方法 |
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CN103614160A (zh) * | 2013-12-13 | 2014-03-05 | 海南汉地阳光石油化工有限公司 | 一种重质润滑油基础油生产系统及生产方法 |
CN105219427B (zh) * | 2014-06-16 | 2017-08-25 | 中国石油化工股份有限公司 | 一种润滑油基础油的加工方法 |
CN107474878A (zh) * | 2017-09-29 | 2017-12-15 | 江苏天时新材料科技有限公司 | 一种基础油的加工方法 |
CN109181767A (zh) * | 2018-09-26 | 2019-01-11 | 海南汉地阳光石油化工有限公司 | 一种高速发动机基础油的制备方法 |
CN114341318A (zh) * | 2019-08-12 | 2022-04-12 | 雪佛龙美国公司 | 用于提高基础油产率的工艺 |
CN112023960A (zh) * | 2020-07-20 | 2020-12-04 | 中国科学院大连化学物理研究所 | 催化剂组合物及由丙烷脱沥青油生产高粘度润滑油基础油的方法 |
CN112126463A (zh) * | 2020-07-20 | 2020-12-25 | 中国科学院大连化学物理研究所 | 高粘度润滑油基础油及其制备方法 |
WO2022100426A1 (zh) * | 2020-11-12 | 2022-05-19 | 中国石油天然气股份有限公司 | 异构脱蜡催化剂及其制备方法与生产润滑油基础油的方法 |
CN113088333A (zh) * | 2021-03-15 | 2021-07-09 | 中海油惠州石化有限公司 | Api ⅲ类润滑油基础油及其生产方法 |
Also Published As
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CA2810438A1 (en) | 2012-03-15 |
EP2615155A1 (en) | 2013-07-17 |
KR20140032336A (ko) | 2014-03-14 |
WO2012031449A1 (zh) | 2012-03-15 |
EA201390349A1 (ru) | 2013-08-30 |
US20130253238A1 (en) | 2013-09-26 |
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