CN1516732A - 微晶蜡的制备方法 - Google Patents

微晶蜡的制备方法 Download PDF

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CN1516732A
CN1516732A CNA028120183A CN02812018A CN1516732A CN 1516732 A CN1516732 A CN 1516732A CN A028120183 A CNA028120183 A CN A028120183A CN 02812018 A CN02812018 A CN 02812018A CN 1516732 A CN1516732 A CN 1516732A
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A·赫克
���dz�
H·沙登伯格
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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
    • C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
    • C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
    • C10G45/62—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing platinum group 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
    • C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/42—Refining of petroleum waxes
    • C10G73/44—Refining of petroleum waxes in the presence of hydrogen or hydrogen-generating compounds
    • 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
    • C10G2300/1022—Fischer-Tropsch products
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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
    • C10G2300/301—Boiling range
    • 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
    • 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

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Abstract

一种微晶蜡的制备方法，通过在加氢异构化条件下，使包含至少80wt％的正链烷烃并且凝点高于60℃的进料与包含贵金属和多孔二氧化硅－氧化铝载体的催化剂接触。

Description

微晶蜡的制备方法
本发明涉及一种微晶蜡的制备方法。
通过对沸点在基础油范围内的石油馏分溶剂脱蜡来制备微晶蜡产品是已知的。这些方法的实例在石油手册(The Petroleum Handbook)，第6版，Elsevier，1983，第5章第265页中有述。
由得自于费-托(Fischer-Tropsch)法的产品制备蜡也是已知的，如在“由天然气生产硬蜡的方法和质量以及应用这种蜡所形成的HMA的性能(Manufacturing and quality aspects of producing hardwaxes from natural gas and the resulting HMA performanceobtained when using such a wax)”，Naidoo P.，Watson M.D.，1994 Hot Melt Symposium，TAPPI Proceedings，第165-170页中所述的。
基于费-托产品的这种蜡的缺点在于太硬而难以被用于如特种热熔性粘合剂、PVC生产中的润滑剂、口香糖、石油凝胶、药物制品、化妆品、织物浸渍和纸涂层应用中。蜡的硬度可以通过IP 376方法来测量。使用该方法测得的商购费-托衍生蜡在43℃下的PEN值通常在0.2-0.6mm之间。
本发明的一个目的是提供一种微晶蜡的制备方法，该微晶蜡具有所需性质，特别是其PEN值(IP 376)在43℃下大于0.8mm。
该目的通过以下方法来实现。通过在加氢异构化条件下，使包含至少80wt％的正链烷烃并且凝点高于60℃的进料与包含贵金属和多孔二氧化硅-氧化铝载体的催化剂接触来制备微晶蜡。
优选的加氢异构化条件应使进料中少于10wt％、更优选少于5wt％的沸点高于370℃的化合物被转化成沸点低于370℃的产品。温度适宜为200-400℃，优选为250-350℃。氢分压适宜为10-100巴，优选为30-60巴。重量小时空速适宜为0.5-5kg/l/h。
存在于催化剂中的贵金属优选是铂、钯或所述金属的组合。催化剂中贵金属的含量适宜为0.1-2wt％，优选为0.2-1wt％。
所述催化剂载体可包括任何合适的无定形二氧化硅-氧化铝。该无定形二氧化硅-氧化铝优选含有2-75wt％的氧化铝，更优选含有10-60wt％的氧化铝。非常适用于制备该催化剂载体的无定形二氧化硅-氧化铝产品含有45wt％二氧化硅和55wt％氧化铝，并且是可商购得到的(如Criterion Catalyst Company，USA)。
该无定形二氧化硅-氧化铝载体更优选具有一定的大孔孔度。该载体的大孔率适宜地为5％体积-50％体积，其中大孔率被定义为直径大于100nm的孔的体积百分数。更优选该载体的大孔率为至少10％体积，甚至更优选为至少15％体积，最优选为至少20％体积。用于本方法的特别优选的催化剂包含大孔率为至少25％体积的载体。包含大孔率高的载体的催化剂可能具有缺陷，即催化剂抗碎裂能力低。因此，该大孔率优选不大于40％体积，更优选不大于38％体积，甚至更优选不大于35％体积。该催化剂的侧壁碎裂强度适宜为大于75N/cm，更优选为大于100N/cm。该催化剂的主体碎裂强度适宜为大于0.7MPa，更优选为大于1MPa。
使用测量催化剂的孔体积分布的标准测试方法，通过压汞孔隙法(Mercury Intrusion Porosimetry)，ASTM D 4284-88，在最大压力为4000巴下，并假定汞的表面张力为484达因/cm及与无定形二氧化硅-氧化铝的接触角为14°时测定的孔体积为总的孔体积。由上述方法测得的该载体的总的孔体积通常为0.6-1.2ml/g，优选为0.7-1.0ml/g，更优选为0.8-0.95ml/g。
可以意识到总的孔体积的大部分被孔径小于100nm的中孔和微孔所占据。典型地，这些中孔和微孔的大部分孔径为3.75-10nm。优选地，总孔体积的45-65％体积被孔径为3.75-10nm的孔所占据。
除了无定形二氧化硅-氧化铝以外，该载体还可包含一种或多种粘合剂材料。适合的粘合剂材料包括无机氧化物。无定形的和晶体粘合剂均可使用。粘合剂材料的实例包括二氧化硅、氧化铝、粘土、氧化镁、二氧化钛、氧化锆及其混合物。二氧化硅和氧化铝是优选的粘合剂，氧化铝是特别优选的。如果将粘合剂加入催化剂的话，以载体的总重量计，该粘合剂的存在量优选为5-50wt％，更优选为15-40wt％。对于本发明的方法来说，包含不含粘合剂的载体的催化剂是优选的。上述优选催化剂可以通过如EP-A-666894中所述的方法得到。此外，适用的催化剂在WO-A-200014179、EP-A-532118、EP-A-587246、EP-A-532116、EP-A-537815和EP-A-776959中有述。
所述进料包括至少80wt％，优选至少85wt％的正链烷烃。该进料的凝点高于60℃，优选高于90℃，甚至更优选高于95℃。熔化温度及凝点的上限适宜为低于125℃。按照IP 376测定的在43℃下的PEN值优选小于0.7mm。通过ASTM D 721测定的油含量通常较低，如小于1wt％，更典型地小于0.5wt％。在150℃下进料的运动粘度优选大于7cSt。为了不使催化剂失活，进料的硫含量适宜小于0.1ppm。
此种优选进料适宜地在费-托合成中得到。该方法能够制备具有高含量正链烷的馏分。该方法的实例有所谓的工业Sasol法、工业ShellMiddle Distillate法或非工业的Exxon法。这些和其它方法如在EP-A-776959、EP-A-668342、US-A-4943672、US-A-5059299、WO-A-9920720中有更详细的描述。制备本发明方法进料的优选费-托法在WO-A-9934917中有述。该方法由于其产生的费-托产品包含足够量的凝点高于60℃及更高的馏分而是优选的。
可以作为原料的可商购的费-托衍生蜡产品的例子如在“Shell中间馏分合成产品的市场(The Markets for Shell Middle DistillateSynthesis Products)”，Peter J.A.Tijm，Shell International GasLtd..Alternative Energy’95，Vancouver，Canada，5月2-4，1995中所述的SX100及由Schümann Sasol Ltd(SA)投入市场的Paraflint H1。
在费-托法中直接得到的合成产品优选被加氢以除去该产品中的任何氧化物，并使该产品中存在的任何烯属化合物饱和。该加氢处理如EP-B-668342中所述的。用于本发明产品的进料能够通过蒸馏或任何其它适当的分离技术将低沸点化合物和任选的高沸点化合物从费-托法产品中分离出来而得到。
通过本发明方法以及任选在脱油步骤后得到的微晶蜡可用于前述应用中。该蜡可用作PVC(聚氯乙烯)处理中的润滑剂，如用于硬质PVC挤出物。该蜡还可用作聚乙烯母炼胶的载体蜡。另外已经发现该蜡产品与进料相比，与极性化合物的相容性更好。例如，该蜡产品与极性颜料的相容性更好。
本发明还涉及软微晶蜡，据信其是具有以下性质的新型蜡。通过ASTM D 938测定费-托衍生蜡的凝点为85-120℃，更优选为95-120℃，按照IP 376测定的43℃下的PEN大于0.8mm，优选大于1mm。该蜡进一步的特征在于其优选包含小于1wt％的芳族化合物和小于10wt％的环烷类化合物，更优选为小于5wt％的环烷类化合物。该蜡中的支链链烷烃的摩尔百分数优选大于33，更优选大于45，并低于80mol％，这是通过C13NMR测定的。该方法确定蜡的平均分子量，随后确定具有甲基支链的分子的摩尔百分数、具有乙基支链的分子的摩尔百分数、具有C3支链的分子的摩尔百分数和具有C4 +支链的分子的摩尔百分数，其假设是每个分子的支链不多于1个。支链链烷烃的mol％是这些单个百分数的总和。该方法计算在蜡中分子中平均只有一个支链的分子的mol％。实际上可能存在支链多于1个的链烷烃分子。因此由不同方法测定的支链链烷烃含量的值将不同。
通过ASTM D 721测定的油含量通常低于2wt％。其下限不是关键的。可以预期大于0.5wt％，但更低的值可以根据获得蜡的方法而实现。最可能的油含量为1-2wt％。蜡在150℃下的运动粘度优选高于8cSt，更优选高于12并低于18cSt。
现在用以下非限制性实施例来描述本发明。
实施例1
由费-托合成产品得到的蜡馏分被连续加料至加氢异构化步骤，该费-托合成产品是使用WO-A-9934917的实施例III的催化剂按其实施例VII得到的。该进料的性质如表1所示。
在加氢异构化步骤中，该馏分与EP-A-532118的实施例1的加氢异构催化剂接触。该加氢异构化步骤是在30巴(绝压)及325℃的温度下进行的。其它条件的选择应使进料转化成沸点低于370℃的产品的转化率低于10wt％。
分析该加氢异构化所得到的产品，结果列于表1中。
                                表1
SX100* ParaflintH1** 进料 产品
凝点(ASTM D 938；℃) 97.3 100 104.5 101.0
滴熔点(ASTM D 127)(℃) 110.0 113.5 116.7 113.4
25℃下PEN(IP 376)(mm) 0.1 0.1 0.1 0.8
43℃下PEN 0.4 0.4 0.2 1.6
65℃下PEN 1.1 1.7 0.7 4.0
油含量(ASTM D 721；wt％) ＜0.1 未测量 ＜0.1 1.6
150℃下运动粘度(ASTM D 445) 7.97 未测量 14 13.8
通过显微镜观察的晶体结构 是 是 是 是
％支链(mol％) 9 11.5 11.1 60***
*SX100是由壳牌马来西亚分公司投入市场的费-托蜡
**Paraflint H1是Schumann Sasol投入市场的费-托衍生蜡
***36mol％单-甲基支链链烷烃分子，8mol％单-乙基支链链烷烃分子，4mol％单-丙基支链链烷烃分子及12mol％C4 +单支链链烷烃分子。

Claims (23)

1.一种微晶蜡的制备方法，该方法通过在加氢异构化条件下，使包含至少80wt％正链烷烃并且凝点高于60℃的进料与包含贵金属和多孔二氧化硅-氧化铝载体的催化剂接触。
2.根据权利要求1的方法，其中进料中少于10wt％的沸点高于370℃的化合物被转化为沸点低于370℃的产品。
3.根据权利要求2的方法，其中进料中少于5wt％的沸点高于370℃的化合物被转化为沸点低于370℃的产品。
4.根据权利要求1-3任一项的方法，其中加氢异构化条件包括温度为250-350℃，氢分压为30-60巴及重量小时空速为0.5-5kg/l/h。
5.根据权利要求1-4任一项的方法，其中所述贵金属是铂、钯或所述金属的组合。
6.根据权利要求1-5任一项的方法，其中无定形二氧化硅-氧化铝载体的大孔率为5vol％-50vol％，其中大孔率定义为直径大于100nm的孔的体积百分数。
7.根据权利要求6的方法，共中大孔率为10-40vol％。
8.根据权利要求1-7任一项的方法，其中无定形二氧化硅-氧化铝载体包含2-75wt％的氧化铝。
9.根据权利要求8的方法，其中所述氧化铝含量为10-60wt％。
10.根据权利要求1-9任一项的方法，其中所述载体的总孔体积为0.6-1.2ml/g。
11.根据权利要求1-10任一项的方法，其中所述进料是通过费-托合成得到的。
12.根据权利要求1-11任一项的方法，其中所述进料的凝点为95-120℃。
13.根据权利要求1-12任一项的方法，其中按照IP 376测定的所述进料在43℃下的PEN大于0.7mm。
14.根据权利要求12-13任一项的方法，其中所得到的微晶蜡的凝点为95-120℃，并且按照IP 376测定的在43℃下的PEN大于0.8mm。
15.根据权利要求14的方法，其中在43℃下的PEN大于1.0mm。
16.一种微晶蜡，其凝点为95-120℃，并且按照IP 376测定的在43℃下的PEN大于0.8mm。
17.根据权利要求16的蜡，其中按照IP 376测定的在43℃下的PEN大于1.0mm。
18.根据权利要求16-17任一项的蜡，其中支链链烷烃的含量大于33wt％。
19.根据权利要求16-18任一项的蜡，其中芳族化合物的含量小于1wt％及环烷类化合物的含量小于10wt％。
20.根据权利要求16-19任一项的蜡，其中通过ASTM D 721测定的油含量低于2wt％。
21.由权利要求1-15任一项的方法得到的蜡或权利要求16-20任一项的蜡在热熔性粘合剂中作为固化剂组分的用途。
22.由权利要求1-15任一项的方法得到的蜡或权利要求16-20任一项的蜡在PVC加工中作为润滑剂的用途。
23.由权利要求1-15任一项的方法得到的蜡或权利要求16-20任一项的蜡在化妆品组合物中作为光泽助剂的用途。
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CN101074320B (zh) * 2006-05-19 2010-10-27 中国石油化工股份有限公司 一种饰品精密铸造模料

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