CN106076359A - 一种油脂加氢脱氧用镍基催化剂 - Google Patents
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Abstract
本发明公开了一种油脂加氢脱氧用镍基催化剂，涉及催化剂制备技术领域，以镍为主活性组分，氧化铜和二氧化锰为助活性组分，纳米氧化铝为载体，其中镍的负载量为10‑20％，铜的负载量为5‑8％，锰的负载量为2‑3％。本发明催化剂具有催化活性高、寿命长且稳定性强的特点，并且载体通过预处理进一步扩大了纳米氧化铝的孔道，使平均孔径达到20nm以上，这样不仅大大增加了活性组分负载量，还能避免因催化剂孔径小造成积碳而使催化剂永久失活的问题。
Description
技术领域：
本发明涉及催化剂制备技术领域，具体涉及一种油脂加氢脱氧用镍基催化剂。
背景技术：
油脂类生物质被认为是富有潜力的可再生资源，主要成分为碳、氢和氧，由饱和的或者不饱和的脂肪酸甘油酯和少量游离的脂肪酸组成。这些脂肪酸碳数分布在C14-C18之间，和相对应的柴油组分相一致，因此将油脂催化转化为燃料油是一种解决能源危机的新途径。目前，油脂脱氧转化为脂肪烃的技术主要有金属硫化催化剂加氢脱氧技术、不含硫的还原态金属加氢脱氧技术以及催化裂化技术。在上述油脂催化转化技术中，金属硫化催化剂的稳定性好，但需要引入含硫的硫化氢等维持催化剂活性，因而容易引入硫污染产物。目前新开发的非硫金属催化剂更加绿色清洁，且反应条件更为温和，但稳定性差、活性低、寿命短。以传统微孔分子筛为载体的催化剂孔道直径小于2nm，而油脂类大分子只能在催化剂表面和孔道口反应，反应物、中间物和产物的扩散首先，容易造成积碳而使催化剂永久失活。
发明内容：
本发明所要解决的技术问题在于提供一种活性高、寿命长且稳定性与抗积碳能力强的油脂加氢脱氧用镍基催化剂。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种油脂加氢脱氧用镍基催化剂，以镍为主活性组分，氧化铜和二氧化锰为助活性组分，纳米氧化铝为载体，其中镍的负载量为10-20％，铜的负载量为5-8％，锰的负载量为2-3％。
其制备方法包括如下步骤：
(1)载体预处理：将纳米氧化铝加入2-3倍重量的质量浓度10％氯化铵水溶液中，充分分散后静置30-60min，并于微波频率2450MHz、功率700W下微波处理5-10min，过滤，将滤渣于100-110℃下干燥5-8h，再于450-500℃下焙烧3-5h，最后继续升温至800-850℃焙烧2-3h即可；
(2)主活性组分溶液配制：将镍加入3-5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1-2h，最后继续自然冷却至室温，即得主活性组分溶液；
(3)助活性组分溶液配制：将氧化铜和二氧化锰加入3-5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1-2h，最后继续自然冷却至室温，即得助活性组分溶液；
(4)催化剂制备：将上述所制主活性组分溶液和助活性组分溶液充分混合，再加入预处理后的载体，静置20-30min后先于超声频率40kHz、功率50W下超声处理15-30min，再于微波频率2450MHz、功率700W下微波处理5-10min，处理结束后于0-5℃下静置2-3h，然后转入室温下使混合物自然恢复到室温，过滤，将所得滤饼于100-110℃下干燥5-8h，最后于550-600℃下焙烧3-5h后研磨成粉末，即得催化剂。
本发明的有益效果是：本发明通过主活性组分和助活性组分协同负载到纳米氧化铝上制得油脂加氢脱氧用镍基催化剂，该催化剂具有催化活性高、寿命长且稳定性强的特点，并且载体通过预处理进一步扩大了纳米氧化铝的孔道，使平均孔径达到20nm以上，这样不仅大大增加了活性组分负载量，还能避免因催化剂孔径小造成积碳而使催化剂永久失活的问题。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例1
(1)载体预处理：将纳米氧化铝加入3倍重量的质量浓度10％氯化铵水溶液中，充分分散后静置35min，并于微波频率2450MHz、功率700W下微波处理10min，过滤，将滤渣于100-110℃下干燥8h，再于450-500℃下焙烧3h，最后继续升温至800-850℃焙烧3h即可；
(2)主活性组分溶液配制：将镍加入5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1h，最后继续自然冷却至室温，即得主活性组分溶液；
(3)助活性组分溶液配制：将氧化铜和二氧化锰加入5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1h，最后继续自然冷却至室温，即得助活性组分溶液；
(4)催化剂制备：将上述所制主活性组分溶液和助活性组分溶液充分混合，再加入预处理后的载体，静置30min后先于超声频率40kHz、功率50W下超声处理30min，再于微波频率2450MHz、功率700W下微波处理10min，处理结束后于0-5℃下静置2h，然后转入室温下使混合物自然恢复到室温，过滤，将所得滤饼于100-110℃下干燥8h，最后于550-600℃下焙烧5h后研磨成粉末，即得催化剂。
经检测，催化剂中镍的负载量为17％，铜的负载量为6％，锰的负载量为2％。
实施例2
(1)载体预处理：将纳米氧化铝加入3倍重量的质量浓度10％氯化铵水溶液中，充分分散后静置60min，并于微波频率2450MHz、功率700W下微波处理7min，过滤，将滤渣于100-110℃下干燥8h，再于450-500℃下焙烧5h，最后继续升温至800-850℃焙烧2h即可；
(2)主活性组分溶液配制：将镍加入5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1h，最后继续自然冷却至室温，即得主活性组分溶液；
(3)助活性组分溶液配制：将氧化铜和二氧化锰加入5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1h，最后继续自然冷却至室温，即得助活性组分溶液；
(4)催化剂制备：将上述所制主活性组分溶液和助活性组分溶液充分混合，再加入预处理后的载体，静置30min后先于超声频率40kHz、功率50W下超声处理30min，再于微波频率2450MHz、功率700W下微波处理10min，处理结束后于0-5℃下静置2h，然后转入室温下使混合物自然恢复到室温，过滤，将所得滤饼于100-110℃下干燥8h，最后于550-600℃下焙烧5h后研磨成粉末，即得催化剂。
经检测，催化剂中镍的负载量为16％，铜的负载量为5％，锰的负载量为2％。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明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。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (2)
1.一种油脂加氢脱氧用镍基催化剂，其特征在于：以镍为主活性组分，氧化铜和二氧化锰为助活性组分，纳米氧化铝为载体，其中镍的负载量为10-20％，铜的负载量为5-8％，锰的负载量为2-3％。
2.根据权利要求1所述的油脂加氢脱氧用镍基催化剂，其特征在于，其制备方法包括如下步骤：
(1)载体预处理：将纳米氧化铝加入2-3倍重量的质量浓度10％氯化铵水溶液中，充分分散后静置30-60min，并于微波频率2450MHz、功率700W下微波处理5-10min，过滤，将滤渣于100-110℃下干燥5-8h，再于450-500℃下焙烧3-5h，最后继续升温至800-850℃焙烧2-3h即可；
(2)主活性组分溶液配制：将镍加入3-5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1-2h，最后继续自然冷却至室温，即得主活性组分溶液；
(3)助活性组分溶液配制：将氧化铜和二氧化锰加入3-5倍重量的质量浓度20％稀硝酸水溶液中，搅拌下加热至回流状态使其完全溶解，然后自然冷却至55-65℃保温1-2h，最后继续自然冷却至室温，即得助活性组分溶液；
(4)催化剂制备：将上述所制主活性组分溶液和助活性组分溶液充分混合，再加入预处理后的载体，静置20-30min后先于超声频率40kHz、功率50W下超声处理15-30min，再于微波频率2450MHz、功率700W下微波处理5-10min，处理结束后于0-5℃下静置2-3h，然后转入室温下使混合物自然恢复到室温，过滤，将所得滤饼于100-110℃下干燥5-8h，最后于550-600℃下焙烧3-5h后研磨成粉末，即得催化剂。
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