CN106244184B - 一种生物质热解气催化裂解制备btx的方法 - Google Patents

一种生物质热解气催化裂解制备btx的方法 Download PDF

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CN106244184B
CN106244184B CN201610700608.4A CN201610700608A CN106244184B CN 106244184 B CN106244184 B CN 106244184B CN 201610700608 A CN201610700608 A CN 201610700608A CN 106244184 B CN106244184 B CN 106244184B
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metal nitride
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陆强
李文涛
周民星
胡斌
王昕�
郭浩强
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North China Electric Power University
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Abstract

本发明属于生物质能的利用领域，具体涉及一种生物质热解气催化裂解制备BTX(苯‑甲苯‑二甲苯)的方法。本发明是以负载金属氮化物的沸石分子筛为催化剂，以生物质为原料，将生物质在无氧条件下于450～850℃下进行常规热解后将热解气相产物通过装有金属氮化物基催化剂的反应器中进行催化裂解，对热解气进行冷凝即可得到富含BTX的液体产物。

Description

一种生物质热解气催化裂解制备BTX的方法
技术领域
本发明属于生物质能的利用领域，具体涉及一种生物质热解气催化裂解制备BTX的方法。
背景技术
生物质快速热解是一个极为复杂的热化学转化过程，经历大量热解反应路径从而形成复杂的液体产物生物油，生物油中含有多种高附加值的化学品，但含量一般都很低，难以分离提取。因此，为了直接获得富含特定高附加值化学品的生物油，需要对生物质热解过程或者热解产物进行定向调控或转化，从而选择性地促进特定目标化学品的生成并抑制其他液体副产物的生成。
生物质常规热解的产物虽然极为复杂，研究人员发现，当采用沸石分子筛催化剂(HZSM-5、Hβ、HY等)对生物质常规热解气相产物进行催化裂解时，由于沸石分子筛的芳构化效果，可以将多种产物都高效转化为芳香烃类产物，而且由于沸石分子筛的择形性，芳香烃产物中BTX(苯-甲苯-二甲苯)的含量较高，因此有望提供一种新型的BTX制备工艺。然而，研究人员同时也发现，沸石分子筛催化剂的催化性能还有待于改进，主要在于该类催化剂使用时，BTX的产率还较低，而且还伴随着大量多环芳烃的生成(其含量可占芳香烃总含量的近一半)，严重制约了该催化剂的大规模工业应用，因此急需对催化剂进行优化改性以提高其对BTX的选择性并降低对多环芳烃的选择性。
发明内容
本发明的目的在于克服现有技术的不足，提供一种生物质热解气催化裂解制备BTX的方法。
本发明所述方法，具体如下：
以负载金属氮化物的沸石分子筛为催化剂，以木质纤维素类生物质为原料，将生物质在无氧条件下于450～850℃进行热解反应，热解反应的时间不超过50s，而后将热解气通入装有催化剂的反应器中进行催化裂解，反应空速满足200～30000h-1，收集经催化裂解后的热解气，经冷凝后得到富含BTX的液体产物。所谓反应空速，即是：热解气的流速(Nm3/h)与催化剂体积(m3)的比值。
所述负载金属氮化物的沸石分子筛催化剂是以沸石分子筛为载体，金属氮化物为活性成分。
所述负载金属氮化物的沸石分子筛催化剂的沸石分子筛载体是HZSM-5、Hβ、HY中的任意一种。
所述负载金属氮化物的沸石分子筛催化剂的金属氮化物活性成分是W2N、Mo2N、VN、Fe3N中的任意一种。
所述负载金属氮化物的沸石分子筛催化剂中的氮化物的质量百分比为5％～35％；优选的，所述负载金属氮化物的沸石分子筛催化剂中的氮化物的质量百分比为8％～25％。
所述负载金属氮化物的沸石分子筛催化剂的典型制备方法如下，以W2N/HZSM-5为例：
以偏钨酸铵为活性前驱物，HZSM-5为载体，通过等体积浸渍、焙烧和程序升温还原进行制备。将偏钨酸铵溶液等体积浸渍HZSM-5后，经过干燥并在550℃下焙烧获得WO3/HZSM-5前驱体，之后在NH3氛围下程序升温还原，升温程序为：室温～300℃(10℃/min)，300～500℃(0.5℃/min)，500～700℃(1℃/min)，700℃恒温保留2h，之后在NH3氛围下自然冷却至室温获得新鲜W2N/HZSM-5催化剂。将上述新鲜催化剂经O2/N2(O2含量1vol％)室温处理4h，获得钝化W2N/HZSM-5，用于催化生物质制备BTX。其他负载金属氮化物的沸石分子筛催化剂采用相似的方法进行制备。
所述木质纤维素类生物质是以纤维素、半纤维素和木质素为主要组成的生物质原料，包括木材、农作物秸秆、竹材或者草本类生物质。
所述无氧条件是指反应体系维持在惰性无氧保护气体环境下。
所述热解反应的升温速率不低于100℃/s。
本发明的有益效果为：
本发明采用负载金属氮化物的沸石分子筛催化剂，通过对生物质热解气相产物进行催化裂解，制备富含BTX的液体产物。沸石分子筛载体本身具有良好的择形性和芳构化效果，可将生物质热解气相中的不同产物都转化为芳香烃类产物，但同时也会发生结焦和聚合等反应，生成焦炭和多环芳烃等产物；而金属氮化物本身具有一定的加氢功能，当负载于沸石分子筛形成负载型催化剂后，在活性成分和载体的协同作用下，能够显著促进BTX的形成，同时通过抑制聚合等反应的发生从而抑制多环芳烃、其他单环芳烃以及其他有机副产物的生成，由此获得富含BTX的生物油。
具体实施方式
本发明提供了一种生物质热解气催化裂解制备BTX的方法，下面结合具体实施方式对本发明做进一步说明。
下述实施例中的百分含量如无特殊说明均为质量百分含量。
实施例1
取100g干燥的杨木(粒径为0.1～0.3mm)为原料，以W2N/HZSM-5(HZSM-5的硅铝比为25，W2N负载量为12％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将杨木在氮气氛围下680℃快速热解，热解时间20s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为2000h-1，获得的液体产物产率为41.8％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为6.8％。
实施例2
取100g干燥的杨木(粒径为0.1～0.3mm)为原料，以Mo2N/HZSM-5(HZSM-5的硅铝比为25，Mo2N负载量为12％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将杨木在氮气氛围下650℃快速热解，热解时间25s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为1800h-1，获得的液体产物产率为42.3％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为7.3％。
实施例3
取100g干燥的玉米秸秆(粒径为0.1～0.3mm)为原料，VN/Hβ(Hβ的硅铝比为25，VN负载量为10％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将玉米秸秆在氮气氛围下720℃快速热解，热解时间20s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为2200h-1，获得的液体产物产率为38.3％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为6.1％。
实施例4
取100g干燥的竹子(粒径为0.1～0.3mm)为原料，Fe3N/HY(HY的硅铝比为25，Fe3N负载量为15％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将竹子在氮气氛围下630℃快速热解，热解时间25s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为2000h-1，获得的液体产物产率为40.2％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为6.6％。
实施例5
取100g干燥的棉秆(粒径为0.1～0.3mm)为原料，Mo2N/HZSM-5(HZSM-5的硅铝比为25，Mo2N负载量为17％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将棉秆在氮气氛围下700℃快速热解，热解时间20s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为2100h-1，获得的液体产物产率为42.6％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为6.8％。
实施例6
取100g干燥的甘蔗渣(粒径为0.1～0.3mm)为原料，Fe3N/HZSM-5(HZSM-5的硅铝比为25，Fe3N负载量为12％)为催化剂(催化剂研磨至粒径为0.2mm左右)；首先将甘蔗渣在氮气氛围下750℃快速热解，热解时间20s，经气固分离后，将高温热解气直接通入催化剂层，控制热解气在催化剂反应器内的反应空速为2200h-1，获得的液体产物产率为41.7％，通过气相色谱分析其中BTX的含量，计算得知BTX的产率为6.9％。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所做的任何修改，等同替换、改进等，均应包含在本发明的范围之内。

Claims (8)

1.一种生物质热解气催化裂解制备BTX的方法，其特征在于，以负载金属氮化物的沸石分子筛为催化剂，以木质纤维素类生物质为原料，将生物质在无氧条件下于450～850℃进行热解反应，热解反应的时间不超过50s，然后将热解气通入装有催化剂的反应器中进行催化裂解，反应空速满足200～30000h-1，收集经催化裂解后的热解气，经冷凝后得到富含BTX的液体产物。
2.根据权利要求1所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述负载金属氮化物的沸石分子筛催化剂是以沸石分子筛为载体，金属氮化物为活性成分。
3.根据权利要求2所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述负载金属氮化物的沸石分子筛催化剂的沸石分子筛载体是HZSM-5、Hβ、HY中的任意一种。
4.根据权利要求2所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述负载金属氮化物的沸石分子筛催化剂的金属氮化物活性成分是W2N、Mo2N、VN、Fe3N中的任意一种。
5.根据权利要求1所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述负载金属氮化物的沸石分子筛催化剂中的金属氮化物的质量百分比为5％～35％。
6.根据权利要求1所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述木质纤维素类生物质包括木材、农作物秸秆或竹材。
7.根据权利要求1所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述无氧条件是指反应体系维持在惰性无氧保护气体环境下。
8.根据权利要求1所述的一种生物质热解气催化裂解制备BTX的方法，其特征在于，所述热解反应的升温速率高于100℃/s。
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