CN110871084A - 一种非负载型加氢脱氧催化剂及其制备方法 - Google Patents
一种非负载型加氢脱氧催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 21
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 12
- 150000002815 nickel Chemical class 0.000 claims description 10
- 150000002821 niobium Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 9
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical group [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- OPDAZMQZDHDLKT-UHFFFAOYSA-N nickel(2+) niobium(5+) oxygen(2-) Chemical compound [O-2].[Nb+5].[Ni+2] OPDAZMQZDHDLKT-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
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- 239000011363 dried mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 7
- 239000003225 biodiesel Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 6
- 239000010775 animal oil Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 235000015112 vegetable and seed oil Nutrition 0.000 description 5
- 239000008158 vegetable oil Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000006392 deoxygenation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 229910003294 NiMo Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- FEBJSGQWYJIENF-UHFFFAOYSA-N nickel niobium Chemical compound [Ni].[Nb] FEBJSGQWYJIENF-UHFFFAOYSA-N 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8474—Niobium
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
- C11C3/123—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation using catalysts based principally on nickel or derivates
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Abstract
本发明公开了一种非负载型加氢脱氧催化剂及其制备方法,这种具有优异活性和水稳定性的用于制备生物柴油的加氢脱氧催化剂,包括氧化镍NiO和氧化铌Nb2O5,所述氧化镍和氧化铌的摩尔比例为(1‑2):(6‑9),以及一种一步制备非负载型加氢脱氧催化剂的制备方法。极大的提高了催化反应的转化率和选择性,同时催化剂制备过程简单、原料经济性好,便于应用推广。
Description
技术领域
本发明涉及一种非负载型加氢脱氧催化剂及其制备方法,应用于动植物油加氢脱氧制备生物柴油领域。
背景技术
化石能源作为一种不可再生能源,其储量在高速增长的能源需求中逐渐显得捉襟见肘。新世纪以来,化石能源的价格节节攀升,同时化石能源的大量燃烧引发温室气体的巨量排放,以及温室效应引发的冰川融化、全球温度升高、干旱洪涝等自然灾害和其他人们日常生活中常见的雾霾、水质污染等污染问题,使人们对日益严重的环境恶化情况尤为关注。因此开发利用可再生、绿色经济的新型能源的需求越来越高。生物柴油作为一种替代传统石化柴油的液体燃料近年来已经投入使用。然而,这些新型可替代能源的初级产品含氧量很高,个别高达50wt.%,大量含氧化合物的存在,存在如燃烧热低、稳定性差和腐蚀性较强等缺陷,限制了其作为动力能源的大规模使用。
为了解决污染问题,需进一步对其进行催化加氢脱氧精制处理,目前研究较多的脱氧催化剂主要采用:负载型过渡金属硫化型催化剂、负载型贵金属催化剂以及负载型过渡金属还原态催化剂。其中酸性载体负载的过渡金属还原态催化剂以其优异的催化活性、无潜在环境污染、制备成本低等特点,已成为油脂加氢脱氧催化剂的研究热点。然而在反应过程中,作为底物或产物的水会毒化酸性载体表面酸性位从而导致催化剂失活。
动植物油的主要成分是三脂肪酸甘油酯,动植物油加氢脱氧制备出的生物柴油可以与石油柴油以任何比例调和,无硫,无芳烃,不含氧,NOx排放少,环境友好,储存稳定性好,可以作为高十六烷值柴油添加组分使用。因此动植物油加氢脱氧生产制备生物柴油作为一种新型可再生补充与替代燃料而受到人们的青睐。目前,动植物油加氢脱氧反应主要采用硫化态CoMo/Al2O3或NiMo/Al2O3催化剂,这类催化剂具有较高的加氢脱硫和加氢脱氧活性,同时还具有较高的加氢脱氧活性,但缺点是催化剂稳定性差,硫化物易流失、容易失活并且制备过程相对复杂,在现有的反应方案下,对原料的催化转化效果较差,反应产物复杂,副产物较多。
发明内容
为解决现有技术催化剂存在的转化率低,反应产物复杂,产品提纯困难的问题,本发明提供一种具有优异活性和稳定性的耐水酸性用于制备生物柴油的加氢脱氧催化剂。本发明提供一种非负载型加氢脱氧催化剂,包括氧化镍NiO和氧化铌Nb2O5,所述氧化镍和氧化铌摩尔比例为(1-2):(6-9)。
进一步的,还包括无定形态的复合镍铌氧化物NixNbyOz,所述复合镍铌氧化物和氧化铌的摩尔比例为(0.1-0.5):(6-9),所述X、Y和Z为任一数值。所述NixNbyOz是一种复杂的双金属复合氧化物,其构成可以是多种NixNbyOz(X、Y数值可变)双金属复合氧化物组成的混合物,也可能是NixNbyOz(X、Y数值确定)的化合物。
进一步的,所述氧化铌为无定形态氧化铌。
进一步的,采用可溶性镍盐和可溶性铌盐混合、干燥和焙烧的步骤制备。
本发明还提供一种非负载型加氢脱氧催化剂的制备方法,其特征在于,包括以下步骤:
1)可溶性镍盐和可溶性铌盐分别溶于水,再相互混合,搅拌均匀;
2)将镍盐和铌盐的混合溶液加热至60-100℃,搅拌至干燥;
3)将干燥后的混合物置于烘箱中100-150℃干燥10-15h;
4)将混合物在马弗炉中,400-800℃焙烧3-5h,收集反应产物。
进一步的,所述可溶性镍盐为Ni(NO3)2·6H2O、Ni(CH3COO)2·4H2O和NiCO3一种或多种混合物。
进一步的,所述可溶性铌盐为草酸铌铵。
有益效果:
本发明采用浆料法一步制备新型非负载型加氢脱氧催化剂,对比目前广泛采用的过渡金属硫化型催化剂或负载型贵金属催化剂,具有如下有益效果。
1)催化剂制备过程简单、原料经济性好,价格明显低于负载型贵金属催化剂;
2)在催化硬脂酸和油酸的加氢脱氧反应中,催化剂表现出优异的催化性能,反应温和,反应温度介于220-280℃之间,低于常规反应温度280-300℃;
3)相同条件下,反应原料转化率能达到80-90%,反应条件充分的情况下能达到100%;
4)目标产物选择性高,对比现有催化剂70-80%的选择性,该新型非负载型加氢脱氧催化剂能达到80-90%。;
5)该新型非负载型加氢脱氧催化剂参与催化反应的使用量大幅低于现有催化剂,连续运行30-100次之后仍能保持优良的活性,没有明显的能效衰减。
具体实施方式
下面结合实施例对本发明作进一步的描述,以下实施例显示和描述了本发明的基本操作步骤,以及优选比例,在不脱离本发明保护范围的前提下,还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。
实施例一
一种非负载型的加氢脱氧催化剂本体的制备:
1)将0.473gNi(NO3)2·6H2O在搅拌的状态下溶解在50ml去离子水中,将3.1438g草酸铌铵在搅拌状态下溶解在50ml去离子水中;将硝酸镍水溶液缓慢加入到草酸铌铵水溶液中混合搅拌均匀;
2)混合均匀后90℃加热搅拌,12h蒸发掉体系中的水至干燥;
3)将干燥产物放进120℃烘箱中烘干10h;
4)将混合物在马弗炉中,500℃焙烧4h,收集反应产物。
所述马弗炉的升温速率设置为4-10℃/min。
根据上述制备方法,得到一种非负载型的加氢脱氧催化剂,包括氧化镍NiO和氧化铌Nb2O5,所述氧化镍、氧化铌和复合镍铌氧化物摩尔比例为1:4:0.3。
进一步的,所属催化剂在进行催化反应前,在流速为50ml/min氢气流中,设置的升温速率为2℃/min,焙烧温度为400℃,还原焙烧4h。焙烧后温度降至30℃以下时断开氢气,通0.5%的O2/He保护气钝化30min。
实施例二
一种非负载型的加氢脱氧催化剂本体的制备:
1)将0.273g Ni(NO3)2·6H2O在搅拌的状态下溶解在50ml去离子水中,将3.0498g草酸铌铵在搅拌状态下溶解在50ml去离子水中;将硝酸镍水溶液缓慢加入到草酸铌铵水溶液中混合搅拌均匀;
2)混合均匀后90℃加热搅拌,12h蒸发掉体系中的水至干燥;
3)将干燥产物放进120℃烘箱中烘干10h;
4)将混合物在马弗炉中,500℃焙烧4h,收集反应产物。
所述马弗炉的升温速率设置为4-10℃/min。
根据上述制备方法,得到一种非负载型的加氢脱氧催化剂,包括氧化镍NiO和氧化铌Nb2O5,所述氧化镍、氧化铌和复合镍铌氧化物摩尔比例为1:8:0.5。
进一步的,所属催化剂在进行催化反应前,在流速为50ml/min氢气流中,设置的升温速率为2℃/min,焙烧温度为400℃,还原焙烧4h。焙烧后温度降至30℃以下时断开氢气,通0.5%的O2/He保护气钝化30min。
Claims (7)
1.一种非负载型加氢脱氧催化剂及其制备方法,其特征在于:包括氧化镍NiO和氧化铌Nb2O5,所述氧化镍和氧化铌的摩尔比例为(1-2):(6-9)。
2.根据权利要求1所述的一种非负载型加氢脱氧催化剂,其特征在于:还包括无定形态的复合镍铌氧化物NixNbyOz,所述复合镍铌氧化物和氧化铌的摩尔比例为(0.1-0.5):(6-9),所述X、Y和Z为任一数值。
3.根据权利要求1所述的一种非负载型加氢脱氧催化剂,其特征在于:所述氧化铌为无定形态氧化铌。
4.根据权利要求1所述的一种非负载型加氢脱氧催化剂,其特征在于:采用可溶性镍盐和可溶性铌盐混合、干燥和焙烧的步骤制备。
5.根据权利要求1或4所述的一种非负载型加氢脱氧催化剂的制备方法,其特征在于,包括以下步骤:
1)可溶性镍盐和可溶性铌盐分别溶于水,再相互混合,搅拌均匀;
2)将镍盐和铌盐的混合溶液加热至60-100℃,搅拌至干燥;
3)将干燥后的混合物置于烘箱中100-150℃干燥10-15h;
4)将混合物在马弗炉中,400-800℃焙烧3-5h,收集反应产物。
6.根据权利要求4所述的一种非负载型加氢脱氧催化剂,其特征在于:所述可溶性镍盐为Ni(NO3)2·6H2O、Ni(CH3COO)2·4H2O和NiCO3的一种或多种混合物。
7.根据权利要求4所述的一种非负载型加氢脱氧催化剂,其特征在于:所述可溶性铌盐为草酸铌铵。
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