TWI642482B - 氫化處理觸媒、該觸媒之製造方法、以及使用該觸媒之烴油之氫化處理方法 - Google Patents
氫化處理觸媒、該觸媒之製造方法、以及使用該觸媒之烴油之氫化處理方法 Download PDFInfo
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- TWI642482B TWI642482B TW104107550A TW104107550A TWI642482B TW I642482 B TWI642482 B TW I642482B TW 104107550 A TW104107550 A TW 104107550A TW 104107550 A TW104107550 A TW 104107550A TW I642482 B TWI642482 B TW I642482B
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- hydrogenation
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- 238000002360 preparation method Methods 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
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Abstract
本發明課題在於提供一種具有比以往更優異的氫化處理(氫化、脫硫、脫氮)性能的觸媒作為烴油之氫化處理觸媒,以及使用該觸媒之烴油之氫化處理方法。
課題解決手段為一種觸媒,其係在含有週期表第2族金屬氧化物而且以二氧化矽-氧化鋁為主體的無機多孔質擔體中,含有:以氧化物觸媒基準而計為10~40質量%的週期表第6族元素的至少1種、0.5~15質量%的週期表第8~10族元素的至少1種,以及相對於週期表第6族與第8~10族元素的合計莫耳數為0.05~3倍量的有機添加物而成。
Description
本發明關於一種除去烴油所含的硫、氮等的雜質之氫化處理觸媒、該觸媒之製造方法及其利用方法。
近年來,隨著世界性的大氣環境改善動向,作為主要燃料的餾出油的氫化精製用的氫化處理觸媒,非常需要更進一步提升性能。
通常烴油的氫化處理觸媒一般而言是在氧化鋁、二氧化矽等的無機耐熱性擔體擔持鉬與鈷或鎳等的氫化活性金屬成分並且燒成。
然而,近年來為了謀求觸媒性能進一步的提升,如以所例示般,擔體之改質或觸媒金屬之擔持方法等,有文獻提出了各種辦法或提案。
專利文獻1提案了一種在含有鹼土類金屬氧化物0.1~10重量%的鹼土類金屬氧化物-二氧化矽-氧化
鋁擔體上擔持選自週期表6B族、8族元素的活性成分而成的氫化處理觸媒。
然而,由於該觸媒的比表面積高達200m2/g以上,因此其平均細孔直徑窄小,烴分子在觸媒細孔內的擴散變得不足,無法充分對應於廣範圍沸點的餾出油的脫硫,而留下了問題點。
專利文獻2提出了一種進行烴油超深度脫硫的觸媒,其係使第VIB族金屬、第VIII族金屬、磷與有機添加劑存在於慣用的氧化物擔體而成觸媒。
然而,專利文獻2缺乏與擔體改質或觸媒的物理性狀等的最適化有關的具體資訊,依據此文獻的記載,難以開發出脫硫、脫氮活性經過最適化的觸媒。
在專利文獻3中,提出了在含有二氧化矽、氧化鎂、氧化鋁的氧化物擔體擔持週期表第VIa族金屬、第VIII族金屬及二元醇而成的氫化脫硫脫氮用觸媒。
然而,該觸媒所含的氧化鎂非常多,以擔體基準而計為12~35重量%(計算值),而有難以控制以二氧化矽或氧化鋁為基體的擔體的細孔物性或酸度的缺點。
專利文獻4提案了在非晶質的二氧化矽-氧化鋁觸媒支持體含有至少1種金屬、改質劑的碳質供給原料的氫化處理觸媒。
此處可適用的觸媒支持體,例示了二氧化矽-氧化鋁-二氧化鋯、二氧化矽-氧化鋁-氧化釭、二氧化矽-氧化鋁-氧化鈦或二氧化矽-氧化鋁-氧化鎂等,然而關於這種三元
系擔體的具體製法、組成完全沒有揭示。所以,依據此文獻的記載,難以開發出脫硫、脫氮活性經過最適化的觸媒。
〔專利文獻1〕日本特開2000-5601號公報
〔專利文獻2〕日本特開2000-313890號公報
〔專利文獻3〕日本特開2001-310133號公報
〔專利文獻4〕日本特表2012-532212號公報
本發明所欲解決的課題,在於提供一種烴油之氫化處理觸媒,係具有比以往更優異的氫化處理(氫化、脫硫、脫氮)性能的觸媒、其製造方法,以及使用該觸媒之烴油之氫化處理方法。
本發明人等鑑於先前技術的上述問題點,尤其將焦點放在觸媒擔體的細孔表面的效率的改質,與細孔構造的最適化而反覆潛心研究,結果發現,在含有特定量週期表第2族金屬的二氧化矽-氧化鋁擔體擔持氫化活性成分與有機添加物所得到的觸媒,對於烴油的氫化處理極
為有效,而完成了本發明。
亦即本發明為一種烴油之氫化處理觸媒,其係在含有氧化鋁與二氧化矽以及選自週期表第2族金屬中至少1種金屬的無機多孔質擔體擔持選自週期表第6族金屬中至少1種金屬、選自週期表第8~10族金屬中至少1種金屬及有機添加物。
另外,本發明之氫化處理觸媒,是選自週期表第2族金屬中至少1種金屬含量係以氧化物觸媒基準而計為0.3~2質量%,二氧化矽的含量係以氧化物觸媒基準而計為5~10質量%。而且,平均細孔直徑為10~20nm、比表面積為100~160m2/g、全細孔容積為0.3~0.6ml/g。
另外,本發明之烴油之氫化處理觸媒之製造方法,是在含有氧化鋁與二氧化矽以及選自週期表第2族金屬中至少1種金屬的水合物在730~860℃下煅燒所得到的無機多孔質擔體中含浸含有選自週期表第6族金屬中至少1種金屬、選自週期表第8~10族金屬中至少1種金屬及有機添加物的含浸液,並在以使質量減少比例成為3~60質量%的方式使有機添加物殘存於觸媒上的條件下進行乾燥。
此外,本發明之烴油之氫化處理方法,是使烴油與本發明之氫化處理觸媒在反應溫度300~450℃、氫分壓1~20MPa、液體空間速度0.1~10hr-1、氫/油比50~1,200Nm3/kl的條件下接觸。
藉由使用本發明之氫化處理觸媒,比以往的觸媒更能夠由烴油有效除去硫、氮等的雜質,而提升烴油等級。
以下針對本發明作詳細說明,本發明之觸媒所使用的擔體是以二氧化矽-氧化鋁作為基體,並含有特定量的週期表第2族金屬氧化物。
二氧化矽原料可使用各種矽化合物,例如鹼金屬矽酸鹽、烷氧基矽烷、四氯化矽、正矽酸酯、聚矽氧、二氧化矽溶膠、二氧化矽膠體等。
另外,氧化鋁原料可採用鋁的氫氧化物(拜耳石、三水鋁石、硬鋁石、水鋁礦、擬水鋁礦等)、氯化物、硝酸鹽、硫酸鹽、烷氧化物、鋁酸鹼金屬鹽、其他無機鹽、有機鹽或氧化鋁溶膠。
另一方面,週期表第2族金屬氧化物的原料物質可列舉氧化物、鹵化物(氟化物、氯化物、溴化物、碘化物,以下同樣)、氫氧化物、氫化物、硝酸鹽、碳酸鹽、硫酸鹽、有機酸鹽等。週期表第2族元素可適用鎂、鈣、鍶、鋇,而以鎂、鈣為佳,從活性的觀點看來,特佳為鎂。
二氧化矽-氧化鋁-週期表第2族金屬氧化物擔體,可藉由將共沉法或混練法等所調製出的含有第2族金屬的二氧化矽-氧化鋁水合物燒成而得到。
前述水合物可藉由各種方法來調製,例如二氧化矽、氧化鋁之原料與第2族金屬化合物的共沉;氧化鋁水合物、矽化合物與第2族金屬化合物的混練;氧化鋁-第2族金屬的水合物與矽化合物的混合;或矽化合物-第2族金屬之混合物與氧化鋁水合物的混練等。
在二氧化矽-氧化鋁-週期表第2族金屬氧化物擔體擔持氫化活性金屬或有機添加物,並使其觸媒化,然後其中二氧化矽成分以氧化物觸媒基準而計為3~12質量%,宜為5~10質量%,較佳為6~9質量%。
另一方面,週期表第2族金屬氧化物以氧化物觸媒基準而計為0.3~2質量%,宜為0.4~1.8質量%,較佳為0.5~1.5質量%。
含有週期表第2族金屬的二氧化矽-氧化鋁水合物,可為了因應必要控制細孔構造而添加鹽酸、硫酸、硝酸、有機酸(蟻酸、醋酸、丙酸、草酸、丙二酸、蘋果酸、酒石酸、檸檬酸、葡萄糖酸等)、氨、氫氧化鈉等的水溶液,進行解膠操作,並為了提升成形性而加以混練,然後成形為所希望的形狀(顆粒、球、擠出成形體等)。
成形物通常在空氣中並在730~860℃(並非氣體環境溫度,而是成形物的物質溫度)的溫度下,宜為740~850℃,較佳為750~840℃,煅燒0.1~3小時,宜為0.5
~2小時,而製成擔體。
對於上述步驟所得到的擔體添加氫化活性成分與有機添加物,並實施乾燥處理,而將該等擔持在擔體上。
添加方法並無特別限制,可適用例如含浸法、塗佈法、噴灑法等各種工業方法,而從作業性或添加效率的觀點看來,以含浸法為佳。含浸法的操作手法,例如吸附法、平衡吸附法、填孔法、Incipient Wetness法、蒸發乾燥法、噴霧法等,任一者皆可適用於本發明,而從作業性的觀點看來,以填孔法為佳。
氫活性成分或有機添加物的添加的順序亦並未受到特別限定,可逐次或同時添加。在含浸法的情況下,可使用將各成分溶於各種極性有機溶劑、水或水-極性有機溶劑混合物的溶液,而最佳的溶劑為水。
所擔持的氫化活性成分之中週期表第6族元素,可選自鉻、鉬、鎢的至少1種。這些元素可單獨使用,此情況下,從經濟性或活性的觀點看來,宜為鉬、鎢,尤其以鉬為佳。
另外還可因應原料油的反應性或反應裝置的操作條件而組合使用。在組合的情況下,可例示鉻-鉬、鉻-鎢、鉬-鎢、鉻-鉬-鎢。
全部的週期表第6族元素氧化物的合計擔持量係以氧
化物觸媒基準而計為10~40質量%,宜為15~35質量%、更佳為20~30質量%。在未滿10質量%的情況,觸媒活性低,如果超過40質量%,則活性也並不會增加。
週期表第6族元素的原料可列舉鉻酸鹽、鉬酸鹽、鎢酸鹽、三氧化物、鹵化物、異聚酸、異聚酸鹽等。
氫化活性成分的週期表第8~10族元素可列舉鐵、鈷、鎳。這些元素分別可單獨使用,從經濟性或活性的觀點看來,以鈷、鎳為佳。
此外,還可因應原料油的反應性、反應裝置的操作條件而組合使用。在組合的情況下,可例示鐵-鈷、鐵-鎳、鈷-鎳、鐵-鈷-鎳。
全部的週期表第8~10族元素氧化物的合計擔持量係以氧化物觸媒基準而計為0.5~15質量%,宜為1~10質量%、更佳為2~6質量%。在擔持量未滿0.5質量%的情況,觸媒活性不足,如果超過15質量%,則活性也並不會增加。
擔持所使用的鐵、鈷、鎳的化合物,可採用氧化物、氫氧化物、鹵化物、硫酸鹽、硝酸鹽、碳酸鹽、有機酸鹽等。
在調製氫化活性成分的含浸溶液的情況下,週期表第6族元素、週期表第8~10族元素分別可單獨調製,或可將兩者混合製成均勻溶液。
在氫化活性成分的含浸溶液中,亦可因應必要為了調整溶液的pH、提升液體安定性或觸媒的氫化活
性而添加氨水、過氧化氫水溶液、硝酸、硫酸、鹽酸、磷酸、氫氟酸等。
此外,磷酸亦可作為觸媒成分來添加,此情況下,添加量範圍以氧化物觸媒基準而計,磷氧化物為0.5~15質量%,宜為1~10質量%,更佳為2~8質量%。可添加的磷酸可列舉正磷酸、焦磷酸、偏磷酸、膦酸、二膦酸、膦酸、聚磷酸或該等的有機鹽、無機鹽等。
此外,磷酸除了添加至氫化活性成分的含浸液以外,還可在二氧化矽-氧化鋁-週期表第2族金屬氧化物擔體的調製過程中使其含有添加量的一部分或總量。
有機添加物是如以下所表示般的水溶性有機化合物,可選自多元醇類與該等的醚類、多元醇類或醚類之酯類、糖類、羧酸類或該等的鹽類、胺基酸類或該等的鹽類、各種螯合劑等。
多元醇類與該等的醚類,可例示乙二醇、二乙二醇、三乙二醇、丙二醇、異丙二醇、二丙二醇、三丙二醇、丁二醇(1,2-、1,3-、1,4-、2,3-)、戊二醇(包括例如1,5-、其他的異構物)、3-甲基-1,5-戊二醇、新戊二醇、己二醇(包括例如1,2-、1,6-、其他的異構物)、己二醇、聚乙烯醇、聚乙二醇(平均分子量200~600)、聚丙二醇(只限於水溶性)、甘油、三羥甲基乙烷、三羥甲基丙烷、己三醇(包括例如1,2,6-、其他的異構物)、赤藻糖醇、季戊四醇等的多元醇類與該等的醚類(甲基、乙基、丙基、異丙基、丁基、異丁基、第二丁基、第三丁
基或選自該等的任意組合的單醚、二醚、三醚且具有水溶性的物質)。
多元醇類或醚類的酯類,可例示上述多元醇類或前述醚類的酯類(蟻酸、醋酸等的單酯、二酯、三酯且具有水溶性的物質)。
糖類可例示葡萄糖、果糖、異性化糖、半乳糖、麥芽糖、乳糖、蔗糖、海藻糖、澱粉、糊精、果膠、肝醣、卡特蘭多醣等的糖類。
羧酸類或該等的鹽類可例示蟻酸、醋酸、丙酸、草酸、丙二酸、琥珀酸、馬來酸、富馬酸、酒石酸、檸檬酸(酐、單水合物)、蘋果酸、葡萄糖酸、戊二酸等的羧酸類或該等的鹽類。
胺基酸類或該等的鹽類可例示天門冬胺酸、丙胺酸、精胺酸、甘胺酸、麩胺酸等的胺基酸類或該等的鹽類。
各種螯合劑可例示乙二胺(EDA)、二乙三胺(DETA)、三乙四胺(TETA)、四乙五胺(TEPA)、五乙六胺(PEHA)、乙二胺四醋酸(EDTA)、羥乙基乙二胺三醋酸(HEDTA)、二乙三胺五醋酸(DTPA)、三乙四胺六醋酸(TTHA)、羥乙基亞胺基二醋酸(HIDA)、1,3-丙烷二胺四醋酸(PDTA)、1,3-二胺基-2-羥基丙烷四醋酸(PDTA-OH)、反-1,2-環己二胺四醋酸(CyDTA)、乙二醇醚二胺基四醋酸(GEDTA)、氮基三醋酸(NTA)、二羥乙基甘胺酸(DREG)、(S,S)-乙
二胺-N,N'-二琥珀酸(EDDS)等的各種螯合劑。
上述有機添加物可單獨或適當地組合使用。
有機添加物的添加量為週期表第6族元素及週期表第8~10族元素合計莫耳數的0.05~3倍量,宜為0.08~2.8倍量,特佳為0.1~2.5倍量。在未滿0.05倍莫耳的情況,並沒有觀察到觸媒性能的提升效果。如果超過3倍莫耳,活性也沒有增加得更高。
此外,有機添加物的添加與氫化活性成分的添加之間的關係,也就是氫化活性成分與有機添加物的添加順序,並無限制。亦即,有機添加物可在氫化活性成分的添加前或添加後以另一個溶液的方式添加,或可與氫化活性成分一起製成均勻溶液而同時添加。此外,氫化活性成分溶液、有機添加物溶液或該等的均勻溶液,還可因應溶液的黏度或擔體的細孔容積(吸水量)一起添加或分成多次添加。
在氫化活性成分、有機添加物的添加結束,然後實施後述乾燥處理,而製作出週期表第6族元素、週期表第8~10族元素及有機添加物擔持在擔體上的觸媒完成品。在擔持上述成分時,藉由停止在乾燥處理,不進行燒成,可得到活性比以往的燒成觸媒更優異的觸媒。
在此乾燥處理中,希望有機添加物不會改變基本骨架構造(不考慮結晶水、氫離子、氫氧化物離子、銨離子等的加成或脫離),並且至少其一部分與氫化活性成分發生交互作用(分子間作用力、氫鍵、共價鍵、離子鍵、配位
鍵等)而殘存。
有機添加物的殘存比例的基準,是將觸媒完成品在空氣中並在550℃下加熱1小時的質量減少比例,係以在3~60質量%的範圍內為佳,宜為4~55質量%,特佳為5~50質量%。在質量減少比例未滿3質量%的情況下,所擔持的有機添加物會揮發、分解等,而與氫化活性金屬成分的交互作用不足,並沒有觀察到觸媒活性的提升。在超過60質量%的情況,預硫化步驟時產生大量的水,有機添加物會流出,對於觸媒活性的提升並無幫助。
只要能夠保持上述有機添加物與氫化活性成分的交互作用,則乾燥方法並無特別限制。適合使用例如在空氣中或惰性氣體中的對流傳熱乾燥(熱風乾燥)、輻射傳熱乾燥(紅外線、遠紅外線乾燥)、傳導傳熱乾燥、微波乾燥、冷凍乾燥或減壓乾燥等的各種工業方法。乾燥條件並未受到特別限定,可依照有機添加物的揮發、分解條件適當地設定。
最簡便的乾燥方法為熱風乾燥,此情況下,乾燥條件為例如在空氣中或惰性氣體(氮氣、惰性氣體、二氧化碳、低氧氣體環境等)中,以及如上述般不會改變有機添加物的基本骨架的溫度或時間,可列舉例如在30~250℃下(並非氣體環境溫度,而是乾燥物的物質溫度),宜為50~220℃,較佳為80~180℃,更佳為90~150℃,進行0.1~3小時。此外,本發明之觸媒在製造階段的物質溫度,是藉由業界人士所使用的任意手段,例如熱電偶所能
夠測得的溫度。
為了使完成的觸媒發揮出良好的觸媒性能,希望具有以下的物性、細孔構造。亦即,平均細孔直徑為9~20nm,宜為10~18nm,較佳為11~16nm。在平均細孔直徑未滿9nm的情況,烴油在細孔內的擴散不充分,若超過20nm,則比表面積降低,因此觸媒性能會降低。
另外,全細孔容積宜為0.3~0.6ml/g,較佳為0.4~0.5ml/g。在0.3ml/g以下的情況,烴油在細孔內的擴散不充分,在超過0.6ml/g的情況下,將觸媒填充至反應器時,觸媒的絕對質量變輕(觸媒活性成分量減少),因此不會表現出足夠的觸媒性能。
此處,表示觸媒細孔均勻度的指標為直徑在平均細孔直徑±1.5nm的範圍的細孔的容積比例,希望為相對於全細孔容積具有20~60%的細孔構造,宜為22~58%。在未滿20%的情況,對於反應沒有幫助的微小細孔或表面積低的大細孔的比例增加,在超過60%的情況,分子較大的烴油在細孔內擴散會受到阻礙,而導致觸媒活性的降低。此外,本發明之觸媒的細孔徑分布為以平均細孔直徑或其附近為中心的單峰性的分布。
比表面積希望為100~170m2/g,較佳的範圍為110~160m2/g,更佳為115~150m2/g。在未滿100m2/g的情況,觸媒性能不足,若超過170m2/g,則平均細孔直徑太
小,因此在反應中細孔阻塞等容易發生。
此外,細孔構造(細孔容積、平均細孔直徑、細孔徑分布等)的值是藉由水銀壓入法(接觸角140°、表面張力480dyn/cm)求得,比表面積的值是藉由BET法求得。觸媒完成品的細孔構造、比表面積的測定或氫化活性成分的擔持量,在定量時,是將觸媒完成品在空氣中並在450℃下處理1小時,除去水分或有機物,以此作為測定對象,將此處所得到的分析、測定值轉換為以氧化物觸媒為基準的值。此外,氫化活性成分或擔體構成成分的定量是使用螢光X光分析裝置。
此外,觸媒通常是在實施預硫化操作之後使用,而此預硫化操作可在反應塔內或反應塔外實施。
預硫化方法,適合採用在加熱狀態、氫氣體環境下,使用含有硫成分的燈油或輕油餾出物,或在這些油中適量添加二硫化碳、丁硫醇、二甲基二硫(DMDS)、二第三壬基聚硫醚(TNPS)等的硫化劑來進行的液相硫化;或在加熱氫氣流中,使用硫化氫或二硫化碳作為硫化劑來進行的氣相硫化法等。
利用本發明之觸媒進行氫化處理的處理對象的烴油,是依據ASTM D-2887或D-2887擴展方法,90%沸點溫度為560℃以下,宜為540℃以下,初餾點為100℃以上,宜為150℃以上的餾出油。
具體而言,主要可例示石油系的石油腦、直餾燈油、直餾輕油、重質輕油、減壓輕油、重質減壓輕油等,還包括由氫化分解裝置、熱分解裝置或流動接觸分解裝置所得到的燈輕油餾出物(輕循環油或輕石油焦制氣油等)或重油直接脫硫裝置所產生的燈輕油餾出物,以及來自煤炭或來自動植物的生質量且相當於燈輕油的餾出物,以上列舉的餾出成分的任意混合油。
此外,處理的原料油中,釩或鎳這些金屬成分希望為5質量ppm以下,宜為1質量ppm以下,殘留碳成分希望為1質量%以下,宜為0.9質量%以下,而為了滿足前述金屬成分或殘留碳成分的含量,還可在原料餾出油中混入減壓輕油、常壓殘油、減壓殘油、溶劑脫瀝青油、煤炭液化油、頁岩油、瀝青砂油等的重質油進行處理。
本發明之氫化處理觸媒,可使用於藉由固定床、沸騰床、移動床等的反應器使前述烴油在氫的存在下進行氫化、氫化脫硫、氫化脫氮、氫化脫氧、氫化分解、氫化異性化等的各種氫化處理反應。本發明之氫化處理觸媒,較合適的用途為石油系餾出油的脫硫、脫氮,尤其是使燈油或輕油餾出物中的硫成分減低至80質量ppm以下,甚至10質量ppm以下。
在氫化處理裝置中使用的情況下,反應條件一般而言是在氫分壓1~20MPa,宜為3~18MPa、氫/油比50~
1.200Nm3/kl,宜為100~1.000Nm3/kl、液體空間速度0.1~10h-1,宜為0.5~8h-1、反應溫度300~450℃,宜為320~430℃的條件下使用,情形會視原料油種類而定。
藉由以下所示的實施例進一步對本發明具體說明。但是下述實施例完全不會限定本發明。
在加入了溫自來水的槽中添加硫酸鋁、鋁酸鈉及水玻璃,並且混合,而調製出二氧化矽-氧化鋁水合物膠體(二氧化矽/氧化鋁質量比:8.5/91.5)。
由溶液分離出水合物,使用溫水將雜質洗淨除去,然後添加硝酸,接下來加入碳酸鎂(以氧化物觸媒基準,氧化鎂為0.5質量%),使用混練機加熱混練,調整水分比率,然後擠出成形,在空氣中並在780℃下煅燒1.5小時,而得到二氧化矽-氧化鋁-氧化鎂擔體。
在該擔體中含浸含有三氧化鉬、鹼性碳酸鈷、磷酸與作為有機添加物的檸檬酸單水合物、聚乙二醇(平均分子量200)(有機添加物添加量,相對於鉬與鈷的合計莫耳數,檸檬酸單水合物、聚乙二醇分別為0.1倍莫耳、0.3倍莫耳),並且以氧化物觸媒基準而計,三氧化鉬為22質量%、氧化鈷為4質量%、氧化磷為3質量%的水溶
液,在使含浸物的溫度成為120℃的條件下並在空氣中進行熱風乾燥處理2小時,而得到觸媒A。
觸媒A的物性、化學組成揭示於表1。
在實施例1中,將作為有機添加物的檸檬酸單水合物、聚乙二醇(平均分子量200)的使用量改成相對於鉬與鈷的合計莫耳數分別為0.05倍莫耳,除此之外,以與實施例1同樣的方法調製出觸媒B。
將觸媒B的物性、化學組成揭示於表1。
將碳酸鎂的添加量改成以氧化物觸媒基準而計,氧化鎂為0.8質量%,除此之外,以與實施例1同樣的方法調製出觸媒C。
將觸媒C的物性、化學組成揭示於表1。
將碳酸鎂改成碳酸鈣,除此之外,以與實施例1同樣的方法調製出觸媒D。
將觸媒D的物性、化學組成揭示於表1。
在混練機中加入二氧化矽溶膠、擬水鋁礦粉(二氧化
矽/氧化鋁質量比:8.5/91.5),加入碳酸鎂(以氧化物觸媒基準而計,氧化鎂為0.5質量%)、離子交換水、檸檬酸混練後,加熱混練,調整水分比率,然後擠出成形,在空氣中並在780℃下煅燒5小時,得到二氧化矽-氧化鋁-氧化鎂擔體。
在該擔體中含浸含有三氧化鉬、鹼性碳酸鎳、磷酸與作為有機添加物的二乙二醇(有機添加物的添加量相對於鉬與鎳的合計莫耳數為0.4倍莫耳),並且以氧化物觸媒基準而計,三氧化鉬為22質量%、氧化鎳為4質量%、氧化磷為5質量%的水溶液,在使含浸物的溫度成為120℃的條件下,在空氣中進行熱風乾燥處理2小時,而得到觸媒E。
將觸媒E的物性、化學組成揭示於表1。
在加入了溫自來水的槽中,添加硫酸鋁與鋁酸鈉,並且混合,而調製出氧化鋁水合物。由溶液分離出水合物,並使用溫水將雜質洗淨除去,然後添加硝酸,接下來使用混練機加熱混練,調整水分比率,然後擠出成形,在空氣中並在680℃下煅燒1.5小時,而得到氧化鋁擔體。
在該擔體中含浸含有三氧化鉬、鹼性碳酸鈷、磷酸與作為有機添加物的檸檬酸單水合物、聚乙二醇(平均分子量200)(有機添加物添加量相對於鉬與鈷的合計莫耳數,檸檬酸單水合物、聚乙二醇分別為0.1倍莫耳、0.3
倍莫耳),並且以氧化物觸媒基準而計,三氧化鉬為22質量%、氧化鈷為4質量%、氧化磷為3質量%的水溶液,在含浸物的溫度成為120℃的條件下並在空氣中進行熱風乾燥處理2小時,而得到觸媒F。
將觸媒F的物性、化學組成揭示於表1。
在實施例1中,不使用碳酸鎂,並且在890℃下將二氧化矽-氧化鋁水合物的成形物煅燒,除此之外,以與實施例1同樣的方法調製出觸媒G。
將觸媒G的物性、化學組成揭示於表1。
實施例1之中,將碳酸鎂的添加量定為2.1質量%,除此之外,以以與實施例1同樣的方法調製出觸媒H。
將觸媒H的物性、化學組成揭示於表1。
在混練機中加入擬水鋁礦粉、離子交換水、硝酸,充分混練後,加熱混練,調整水分比率,然後擠出成形,在空氣中並在680℃下煅燒1.5小時,而得到氧化鋁擔體。
在該擔體中含浸含有三氧化鉬、鹼性碳酸鎳、磷酸與作為有機添加物的二乙二醇(有機添加物添加量相對於鉬與鎳的合計莫耳數為0.4倍莫耳)並且以氧化物觸媒基準
而計三氧化鉬為22質量%、氧化鎳為4質量%、氧化磷為5質量%的水溶液,在含浸物的溫度成為120℃的條件下並在空氣中進行熱風乾燥處理2小時,而得到觸媒I。
將觸媒1的物性、化學組成揭示於表1。
1)平均細孔直徑±1.5nm的細孔容積相對於全細孔容積的比例
將實施例1~4、比較例1~3的觸媒填充至固定床小型流通反應器,然後利用在表2的輕油中添加二甲基二硫而成的硫化油(總硫成分相當於2.5質量%)進行預硫化,然後改換成表2的原料油,在表3的條件下實施氫化處理測試。
分別以螢光X光法來測定測試中所得到的生成油的硫成分,依據式(1)、(2)求得容量基準的比活性。
將測試結果揭示於表6。
*)依據ASTM D-2887法
上式中,LHSV為液體空間速度、k為反應速率常數、n為反應次數、X為原料油中的硫成分的質量比例、Y為生成油中的硫成分的質量比例。
將實施例5及比較例4的觸媒填充至固定床小型流通反應器,利用在前述表2的輕油中添加二甲基二硫而成的硫化油(總硫成分相當於2.5質量%)進行預硫化,然後改換成表4的原料油,在表5的條件下,進行減壓輕油的氫化處理測試。
對於測試中所得到的生成油以螢光X光法測定硫成分,以氧化分解化學發光法測定氮成分,依據式(3)~(5),求得容量基準的比活性。
將評估結果揭示於表7。
*)依據ASTM D-2887擴展方法
上式中,LKSV為液體空間速度、k為反應速率常數、n為反應次數、X為原料油中的硫或氮成分的質量比例、Y為生成油中的硫或氮成分的質量比例。此外,ln代表自然對數。
脫硫反應次數:1.3次
表6中的能量消耗指數,是指將觸媒的調製過程中所需的燃料、用電量換算為熱量,並將實施例1~4、比較例1~3的數值相對於比較例1的數值之比乘以100倍。
脫硫反應次數:1.3次
脫氮反應次數:1次
表7中的能量消耗指數,是指在觸媒的調製過程中所需的燃料,將用電量換算成熱量,並且將比較例4、實施例5的數值相對於比較例4的數值之比乘以100倍。
由輕油及減壓輕油的氫化處理測試結果(表6、7)可知,使用本發明之二氧化矽-氧化鋁-週期表第2族金屬氧化物擔體的氫化處理觸媒,與使用以往的氧化鋁系擔體的觸媒相比,表現出較優異的氫化脫硫、氫化脫氮活性。
此外,比較例2的觸媒是使用不含週期表第2族金屬的二氧化矽-氧化鋁擔體,而其輕油脫硫活性與實施例大致同等。
然而,為了得到具有與實施例觸媒同樣細孔構造的觸媒,在擔體製造步驟中,必須採用高煅燒溫度,因此在商業製造之中,會有能量成本相對變高的缺點。
本發明之觸媒比以往的觸媒活性更高,在製造層面還能夠抑制能量消耗量,可知為經濟性高的觸媒。
Claims (9)
- 一種烴油之氫化處理觸媒之製造方法,該烴油之氫化處理觸媒為在氧化鋁與二氧化矽以及選自週期表第2族金屬中至少1種金屬所構成的無機多孔質擔體擔持選自週期表第6族金屬中至少1種金屬、選自週期表第8~10族金屬中至少1種金屬及有機添加物,其特徵為:在氧化鋁與二氧化矽以及選自週期表第2族金屬中至少1種金屬所構成的水合物在730~860℃下煅燒所得到的無機多孔質擔體中含浸含有選自週期表第6族金屬中至少1種金屬、選自週期表第8~10族金屬中至少1種金屬及有機添加物的含浸液,並在以使質量減少比例成為3~60質量%的方式使有機添加物殘存於觸媒上的條件下進行乾燥。
- 如請求項1之氫化處理觸媒之製造方法,其中選自週期表第2族金屬中至少1種金屬的含量係以氧化物觸媒基準而計為0.3~2質量%,二氧化矽的含量係以氧化物觸媒基準而計為3~12質量%。
- 如請求項1之氫化處理觸媒之製造方法,其中有機添加物的含量為週期表第6族元素及週期表第8~10族元素合計莫耳數的0.05~3倍量。
- 如請求項1之氫化處理觸媒之製造方法,其中週期表第2族金屬為鎂或鈣,週期表第6族金屬為鉬或鎢,週期表第8~10族金屬為鈷及/或鎳。
- 如請求項1之氫化處理觸媒之製造方法,其中進 一步擔持以氧化物觸媒基準而計0.5~15質量%的磷酸作為觸媒成分。
- 如請求項1之氫化處理觸媒之製造方法,其中有機添加物為選自多元醇類與該等的醚類、多元醇類或醚類之酯類、糖類、羧酸類或該等的鹽類、胺基酸類或該等的鹽類、及螯合劑所構成之群中的至少1種。
- 如請求項1之氫化處理觸媒之製造方法,其中所製造的氫化處理觸媒的平均細孔直徑為9~20nm、比表面積為100~170m2/g、全細孔容積為0.3~0.6ml/g。
- 一種烴油之氫化處理方法,其係使烴油與如請求項1~6中任一項之製造方法所得到的氫化處理觸媒在反應溫度300~450℃、氫分壓1~20MPa、液體空間速度0.1~10hr-1、氫/油比50~1,200Nm3/kl的條件下接觸。
- 如請求項8之氫化處理方法,其中烴油為選自石油系的石油腦、直餾燈油、直餾輕油、重質輕油、減壓輕油及重質減壓輕油所構成之群中的餾出油。
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FR3083142A1 (fr) * | 2018-06-27 | 2020-01-03 | IFP Energies Nouvelles | Catalyseur a base de derives du 1,5-pentanediol et son utilisation dans un procede d’hydrotraitement et/ou d’hydrocraquage |
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