CN106582515A - 一种双峰孔结构的覆碳氧化铝载体及其制备方法 - Google Patents
一种双峰孔结构的覆碳氧化铝载体及其制备方法 Download PDFInfo
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- CN106582515A CN106582515A CN201510664769.8A CN201510664769A CN106582515A CN 106582515 A CN106582515 A CN 106582515A CN 201510664769 A CN201510664769 A CN 201510664769A CN 106582515 A CN106582515 A CN 106582515A
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- carbon
- alumina
- coal
- oxidation
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000011148 porous material Substances 0.000 title claims abstract description 23
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- 238000000034 method Methods 0.000 claims abstract description 34
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C10G2300/10—Feedstock materials
- C10G2300/1096—Aromatics or polyaromatics
Abstract
本发明公开了一种双峰孔结构的覆碳氧化铝载体及其制备方法，该方法步骤如下：(1)将水合氧化铝与碳酸铝铵先混合，然后与碳前身物混和后捏成可塑体，再通过物理成型方法得到成型物，其中，所述水合氧化铝与所述碳酸铝铵的重量比为1：9～9：1，所述水合氧化铝和所述碳酸铝铵的重量总和与所述碳前身物的比为7:3～19:1；(2)将步骤(1)中所述成型物在50-100℃温度下干燥，然后在无氧气氛下经热处理获得双峰孔结构的覆碳氧化铝载体。本发明的双峰孔结构的覆碳氧化铝载体的制备方法工艺简单、利用该方法制备的表面覆碳氧化铝载体具有双峰孔结构，可作为吸附剂和催化剂载体使用。
Description
技术领域
本发明涉及一种双峰孔结构的覆碳氧化铝载体及其制备方法，特别适合作为减压馏分油、焦化蜡油、常压渣油及煤焦油等重质馏分油加氢预处理催化剂载体。
背景技术
石油资源越来越匮乏，原油重质化和劣质化的趋势越来越明显，越来越多的高含硫、高含氮的重质蜡油需要轻质化处理。但目前的催化裂化技术不适于加工硫含量大于0.6％、重金属含量大于20ppm的原料。因此有必要对重质蜡油进行加氢预处理。加氢处理工艺的核心是加氢催化剂。由于重油中的含硫含氮分子大部分以环状大分子形式存在，不仅要求重油加氢催化剂有较高的本征活性，而且要求具有双峰孔结构，以提高大分子孔内扩散速率，使催化剂的活性得到充分发挥。
研究证明Ⅱ型活性相无论对噻吩加氢脱硫还是对吡啶加氢脱氮活性都比I型活性相要高。在传统的氧化铝载体表面覆碳可以减弱‘金属-载体相互作用’，促进更多的‘Ni-Mo-S(Ⅱ)’型活性相。CN200810228425.2提出了一种覆碳加氢催化剂载体的制备方法。首先将拟薄水铝石干胶粉经过挤条成型焙烧后得到无碳氧化铝载体，然后浸渍有机覆碳前身物或覆碳前身物溶液，在无氧气氛下经快速升温碳化后得到了表面覆碳的氧化铝载体。该制备方法中热处理升温过程条件苛刻，难以适应工业化要求；氧化铝的制备一般要经过一次焙烧，再浸渍碳的前身物，然后再经过高温焙烧碳化，操作过程复杂；由于氧化铝载体自身孔体积的限制，该方法制备的含碳载体碳含量一般在10％以下。
对于重油加氢催化剂，具有双峰孔结构的催化剂可以减少大分子扩散阻力，提高催化剂的容碳能力和稳定性。目前制备含双峰孔结构载体的方法主要是加入物理造孔剂，如专利US4448896选用炭黑颗粒为造孔剂，与拟薄水铝石粉混合成型，通过在有氧条件载体的焙烧过程必须为有氧条件下将炭黑氧化为二氧化碳逸出，从而留下一定数量的大孔。对于表面覆碳催化剂而言该方法显然是不适用的，有氧状态下焙烧将会使载体表面碳和物理造孔剂一起烧掉。
发明内容
针对现有技术的不足，本发明提供一种双峰孔结构的覆碳氧化铝载体及其制备方法。该制备方法工艺简单，利用该方法制备的表面覆碳氧化铝载体具有双峰孔结构，可作为吸附剂和催化剂载体使用。
本发明的技术方案具体如下。
本发明提供一种双峰孔结构的覆碳氧化铝载体的制备方法，具体步骤如下：
(1)先将水合氧化铝与碳酸铝铵混合，接着加入碳前身物或碳前身物水溶液混和捏成可塑体，再通过物理成型方法得到成型物，其中，水合氧化铝与碳酸铝铵的重量比为1:9～9:1，水合氧化铝、碳酸铝铵的重量总和与碳前身物干物料的重量比为7:3～19:1；
(2)步骤(1)中得到的成型物经干燥，在无氧气氛下热处理，获得双峰孔结构的覆碳氧化铝载体。
本发明中，步骤(1)中的碳前身物为碳原子数为2-10的有机化合物，其选自含氮有机化合物、含硫有机化合物或含氧有机化合物中的一种或几种，在本发明提供的条件下，上述碳前身物发生脱氢、分解、碳化等复杂反应，在氧化铝表面生成类似碳或焦的产物。
本发明中含氧有机物可为羧基、羰基、羟基部分取代有机化合物。这些物质可为酸类，如醋酸、草酸、丙二酸、酒石酸、柠檬酸等，可为醇类，如乙二醇、丙二醇等，可为醚类，如二甘醇等，也可为酮类、醛类。或者为上述化合物的组合。含氮有机化合物为至少包含一个共价键氮原子的有机化合物，例如乙二胺、己二胺等。含硫有机化合物为至少包含一个共价键硫原子的有机化合物，如硫醇(通式R-SH)、硫醚(通式R-S-R)、二硫化物(通式R-S-S-R)。含硫有机化合物中也可以含有一个或多个羧基、羰基、酯、醚、羟基、巯基的基团取代，如巯基乙酸、巯基丙酸、二巯基丙醇等。除上述含硫化合物外，可以包含砜和亚砜类化合物，如二甲基亚砜、二甲基砜等。
本发明中，水合氧化铝选自拟薄水铝石粉、薄水铝石粉、三水合氧化铝粉、无定形氢氧化铝干胶粉之中的一种或一种以上的混合物，也可含有分子筛、硅、钛、稀土、锆、硼等一种或一种以上的混合物。它们可以是市售产品，也可采用现有任意一种方法制备。
本发明中，碳酸铝铵优选组成为(NH4)mAlO(OH)(HCO3)m·nH2O,其中0<m<1、0<n≤5、优选为0.2≤m≤0.5、0.5≤n≤4。它们可以是市售产品，也可以是任意一种现有方法制备。
本发明中，步骤(1)中的物理成型方法可采用惯用方法，如挤条、压片、滚球等方法，优选挤条法。
本发明中，混合捏成可塑体时，加入胶溶剂；胶溶剂和水合氧化铝的重量比为1:1000～1:10。优选的，胶溶剂和水合氧化铝的重量比为3:200～3:50。胶溶剂的加入，能有效保证成型过程的顺利进行，提高最终制得的双峰孔结构的覆碳氧化铝载体的机械强度。
本发明中，步骤(2)中，热处理的温度为400-900℃，热处理时间为2-8小时，热处理过程升温速率为5-20℃/分钟。
本发明中，步骤(2)中，无氧气氛是密封体系，或者是惰气气氛。惰气气氛选自氮气、氩气、氦气、二氧化碳或水蒸汽中的一种或几种。
本发明还进一步提供根据上述制备方法得到的双峰孔结构的覆碳氧化铝载体，其覆碳量占双峰孔结构的覆碳氧化铝载体总质量的0.1％-15％，孔径为5-20nm的孔占总孔容为45.6％-67.8％，20-100nm的孔占总孔容为2.2％-37.4％。
本发明的有益效果在于：
(1)本发明制备方法所制备的覆碳氧化铝载体具有典型的双峰孔径分布。与现有技术相比，该过程无需加入任何有机物理造孔剂，因此可以选择无氧条件下与覆碳过程同步焙烧，所以制备过程原料均为一次加入，一次混合成型，一次热处理，大大的简化了覆碳氧化铝载体的制备工艺流程，所用设备简洁，能够有效节省经济成本。
(2)通常活性组份与碳载体之间的作用比与氧化铝载体之间的作用小，能提高某些催化剂(例如加氢脱硫)的活性，但碳载体强度低，不能烧焦再生。覆碳氧化铝载体兼具有碳载体的活性高和氧化铝载体强度高易再生的优点。本发明的制备方法中，碳酸铝铵本身纳米棒状结构形成三维堆积孔，同时热处理过程中、碳酸铝铵自身受热分解释放大量的气体逸出而制造得到双峰孔结构。由于该过程无需加入任何有机物理造孔剂，因此载体焙烧过程可以选择无氧条件。经过一次性无氧条件下的热处理即可实现氧化铝载体表面覆碳和载体焙烧。相对于现有载体表面覆碳技术，本发明制备过程中，原料均为一次加入，一次混合成型，一次热处理过程，简化了载体制备过程；得到的载体机械强度高。
附图说明
图1为覆碳氧化铝载体a的孔分布图。
图2为覆碳氧化铝载体c的孔分布图。
图3为覆碳氧化铝载体f的孔分布图。
具体实施方式
下面结合附图和实施例进行详细说明。
实施例1碳酸铝铵A1的制备
称取氢氧化铝干胶粉(烟台恒辉化工有限公司)100g、碳酸氢铵(北京化工厂产品)310g和聚乙二醇(PEG-400，天津光复化学试剂厂)15mL加入600mL去离子水中搅拌，然后再将混合物料转入1L带聚四氟乙烯内衬的密闭压力容器中，100℃沉化8个小时，过滤并将所得白色滤饼于100℃干燥4小时，即得碳酸铝铵A1。
实施例2碳酸铝铵A2的制备
称取硝酸铝(北京化工厂产品)400g、碳酸氢铵300g与聚乙二醇15mL混合研磨20分钟，然后再将混合物料转入1L带聚四氟乙烯内衬的密闭压力容器中，100℃沉化8个小时，过滤并将所得白色滤饼于100℃干燥4小时，即得碳酸铝铵A2。
实施例3-7为本发明的具有双峰孔结构的覆碳氧化铝载体的制备实施例。
实施例3
水合氧化铝与碳酸铝铵的重量比为1:9，水合氧化铝和碳酸铝铵的重量总和与碳前身物与的比为：7:3。称取10g拟薄水铝石干胶粉(上海欣年石化助剂厂)，90克碳酸铝铵A1混合，用30g葡萄糖(天津光复化学试剂厂)作为碳前身物和2.5g浓硝酸(质量分数为69.2％，北京化工厂产品)和80g去离子水配成溶液，再混合搅拌成可塑体，在挤条机上挤成Ф1.2mm的条，在100℃下干燥4小时，然后在N2气氛下由室温经一个小时升至550℃并保持4小时，得到覆碳的氧化铝载体a，其物化性质见表1。
实施例4
水合氧化铝与碳酸铝铵的重量比为9:1，水合氧化铝和碳酸铝铵A1的重量总和与碳前身物与的比为：19:1。称取90g拟薄水铝石干胶粉，10克碳酸铝铵混合，用5g葡萄糖作为碳前身物和2.5g浓硝酸和80g去离子水配成溶液，再混合搅拌成可塑体，在挤条机上挤成Ф1.2mm的条，在100℃下干燥4小时，然后在N2气氛下由室温经一个小时升至550℃并保持4小时，得到覆碳的氧化铝载体b，图1为覆碳氧化铝载体a的孔分布图。其物化性质见表1。
实施例5
称取60g拟薄水铝石干胶粉，40克碳酸铝铵A1混合，用15g葡萄糖作为碳前身物和2.5g浓硝酸和80g去离子水的配成溶液，再混合搅拌成可塑体，在挤条机上挤成Ф1.2mm的条，在100℃下干燥4小时，然后在N2气氛下由室温经一个小时升至550℃并保持4小时，得到覆碳的氧化铝载体c，图2为覆碳氧化铝载体c的孔分布图。其物化性质见表1。
实施例6
将实施案例4中的‘拟薄水铝石’换成‘氢氧化铝干胶粉’，把‘15g葡萄糖’换成‘15g柠檬酸’即成本例，得到覆碳的氧化铝载体d其物化性质见表1。
实施例7
将实施案例4中的‘碳酸铝铵A1’换成‘碳酸铝铵A2’即成本例，得到覆碳的氧化铝载体e其物化性质见表1。
对比例1
采用专利CN200810228425.2中覆碳载体的制备方法：称取130g拟薄水铝石干胶粉，用2.5g浓硝酸和80g去离子水配成的溶液作为胶溶剂，混合搅拌成可塑体，在挤条机上挤成Ф1.2mm的条，在100℃下干燥4小时，然后在空气气氛下550℃焙烧4小时，得到无碳氧化铝载体，用15g葡萄糖作为碳前身物和80g去离子水配成的溶液，等体积浸渍所得无碳氧化铝载体后，在100℃下干燥4小时，然后再N2气氛下由室温经过一个小时升温至550℃并保持4小时，得到覆碳的氧化铝载体f，图3为覆碳氧化铝载体f的孔分布图。其物化性质见表1。
对比例2
首先采用专利US4448896中的方法制备具有大孔结构的氧化铝载体：称取130g拟薄水铝石干胶粉和40g炭黑(牌号N330，山东金能科技有限责任公司)，用2.5g浓硝酸和80g去离子水配成的溶液作为胶溶剂，混合搅拌成可塑体，在挤条机上挤成Ф1.2mm的条，在100℃下干燥4小时，然后在空气气氛下600℃焙烧4小时，得到无碳的大孔氧化铝载体，用15g葡萄糖作为碳前身物和80g去离子水配成的溶液，等体积浸渍所得无碳氧化铝载体后，在100℃下干燥4小时，然后再N2气氛下由室温经过一个小时升温至550℃并保持4小时，得到覆碳的氧化铝载体g，其物化性质见表1。
表1 采用不同方法制备的双峰孔结构的覆碳氧化铝载体物理性质
从实施例的制备过程来看，本发明提供的方法大大的简化了覆碳氧化铝载体的制备工艺流程。上表可以看出，采用本发明提供的方法制备的覆碳氧化铝载体具有明显提高的孔体积和直径为20-100nm的孔体积。
虽然本发明已以较佳实施例揭露如上，然而其并非用以限定本发明，任何熟悉此技术人士，在不脱离本发明的精神和范围内，当可作各种的更动与润饰，因此，本发明的保护范围当以申请的专利范围所界定为准。
Claims (9)
1.一种双峰孔结构的覆碳氧化铝载体的制备方法，其特征在于，具体步骤如下：
(1)先将水合氧化铝与碳酸铝铵混合，接着加入碳前身物或碳前身物水溶液混和捏成可塑体，再通过物理成型方法得到成型物，其中，所述水合氧化铝与所述碳酸铝铵的重量比为1:9～9:1，所述水合氧化铝、所述碳酸铝铵的重量总和与所述碳前身物或所述碳前身物水溶液的干物料的重量比为7:3～19:1；
(2)步骤(1)中得到的所述成型物经干燥，在无氧气氛下热处理，获得双峰孔结构的覆碳氧化铝载体。
2.根据权利要求1所述的制备方法，其特征在于：步骤(1)中所述的碳前身物为碳原子数为2-10的有机化合物，其选自含氮有机化合物、含硫有机化合物或含氧有机化合物中的一种或几种。
3.根据权利要求2所述的制备方法，其特征在于：所述含氮有机物为乙二胺或己二胺；所述含硫化合物选自硫醚、二硫化物、巯基乙酸、巯基丙酸、二巯基丙醇、二甲基亚砜或二甲基砜中任一种；所述含氧化合物选自酸类、醇类，醚类、酮类或醛类中任一种或组合。
4.根据权利要求1所述的制备方法，其特征在于：步骤(1)中，混合捏成可塑体时，加入胶溶剂，所述胶溶剂和水合氧化铝的重量比为1:1000～1:10。
5.根据权利要求4所述的制备方法，其特征在于：所述胶溶剂和水合氧化铝的重量比为3:200～3:50。
6.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，热处理的温度为400-900℃，热处理时间为2-8小时，热处理过程升温速率为5-20℃/分钟。
7.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，所述无氧气氛是密封体系，或者是惰气气氛。
8.根据权利要求7所述的制备方法，其特征在于：所述惰气气氛选自氮气、氩气、氦气、二氧化碳或水蒸汽中的一种或几种。
9.根据权利要求1所述的制备方法得到的双峰孔结构的覆碳氧化铝载体，其特征在于，覆碳量占双峰孔结构的覆碳氧化铝载体总重量的0.1％-15％，孔径为5-20nm的孔占总孔容为45.6％-67.8％，20-60nm的孔占总孔容为2.2％-37.4％。
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| CN108698975A (zh) * | 2016-02-04 | 2018-10-23 | 罗地亚经营管理公司 | 用于制备脂肪胺的大孔催化剂 |
| CN109718747A (zh) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | 双重孔氧化铝载体、脱金属催化剂及其制备方法 |
| CN110935458A (zh) * | 2018-09-25 | 2020-03-31 | 中国石油化工股份有限公司 | 一种加氢脱金属催化剂的制备方法 |
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| CN111097459A (zh) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂及其制备方法 |
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| CN109718747B (zh) * | 2017-10-27 | 2021-10-08 | 中国石油化工股份有限公司 | 双重孔氧化铝载体、脱金属催化剂及其制备方法 |
| CN109718747A (zh) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | 双重孔氧化铝载体、脱金属催化剂及其制备方法 |
| CN108130595B (zh) * | 2017-12-22 | 2020-08-07 | 西南交通大学 | 一种气氛控制制备氧化铝晶须的方法 |
| CN108130595A (zh) * | 2017-12-22 | 2018-06-08 | 西南交通大学 | 一种气氛控制制备氧化铝晶须的方法 |
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| CN110935468A (zh) * | 2018-09-25 | 2020-03-31 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂的制备方法 |
| CN110935468B (zh) * | 2018-09-25 | 2022-06-07 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂的制备方法 |
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| CN110935469B (zh) * | 2018-09-25 | 2022-04-05 | 中国石油化工股份有限公司 | 一种高活性加氢脱金属催化剂的制备方法 |
| CN111097460A (zh) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | 一种渣油加氢脱金属催化剂及其制备方法 |
| CN111097459A (zh) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂及其制备方法 |
| CN111097459B (zh) * | 2018-10-25 | 2022-06-07 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂及其制备方法 |
| CN111097460B (zh) * | 2018-10-25 | 2022-06-07 | 中国石油化工股份有限公司 | 一种渣油加氢脱金属催化剂及其制备方法 |
| CN111686750A (zh) * | 2019-03-13 | 2020-09-22 | 中国石油化工股份有限公司 | 一种加氢脱金属催化剂的制备方法 |
| CN111686748A (zh) * | 2019-03-13 | 2020-09-22 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂的制备方法 |
| CN111686748B (zh) * | 2019-03-13 | 2022-06-07 | 中国石油化工股份有限公司 | 渣油加氢脱金属催化剂的制备方法 |
| CN111821993A (zh) * | 2019-04-18 | 2020-10-27 | 中国石油化工股份有限公司 | 一种重油加氢脱金属催化剂的制备方法 |
| CN111821993B (zh) * | 2019-04-18 | 2022-06-07 | 中国石油化工股份有限公司 | 一种重油加氢脱金属催化剂的制备方法 |
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