CN108620075A - 一种新型生物质基功能纳米材料的制备方法及其应用 - Google Patents
一种新型生物质基功能纳米材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种新型生物质基功能纳米材料的制备方法及其应用。该材料以生物质废弃物为载体,通过在水热炭上负载纳米级的单质镍颗粒,制备了能够应用于市政污泥催化裂解气化的催化剂,该催化剂制备成本低,反应条件温和,催化活性高,具有良好的稳定性和催化寿命,能够显著提高市政污泥的催化气化效果,制备的气化合成气中氢气最高体积分数>80%,焦油催化裂解效率>95%。
Description
技术领域
本发明涉及环境工程和污染物控制技术领域,尤其涉及一种生物质基功能纳米材料的制备及其应用。
背景技术
氢气无毒无臭,燃烧时仅产生水,对环境零污染,是一种理想的绿色清洁能源,广泛应用于化学、食品、交通运输等各个领域。氢能非一次能源,传统制氢方式(天然气重整、电解水、水煤气法等)成本较高,且消耗大量化石能源,污染生态环境。利用廉价且储量丰富的可再生生物质废弃物资源制氢具有广阔的发展潜力。总量急剧增加的市政污泥是我国城镇固体废弃物的重要组成之一。目前处理方式主要为焚烧、填埋以及堆肥,对大气和土壤环境易造成二次污染。因此采用热解气化技术将市政污泥转化为高品质氢能是最有前景的制氢技术之一。以水蒸气为气化介质,进行气化制氢主要存在氢气含量低、焦油副产物含量高等关键问题,限制了该技术的推广应用。本发明针对这两个关键问题,结合我国每年产生大量农业废弃物的特点,提出一种利用廉价农业废弃物制备功能纳米材料的制备方法并用于市政污泥的催化裂解气化制氢。该工艺可有效提高氢气含量并降低焦油含量,既能显著降低制氢生产成本、减少传统化石能源消耗,又为大量赋存的生物质废弃物提供切实可行的解决方案。
发明内容
本发明的目的是针对传统制氢工艺能耗过高、消耗过量化石燃料、环境二次污染严重等问题,结合我国大量赋存的市政污泥、农业废弃物等生物质废弃物,提供一种清洁、可再生的富氢合成气制备新工艺。本发明方法原料廉价可再生,反应条件温和,制备的气化合成气中氢气体积分数高,具有广阔的工业化制氢应用潜力。
为实现本发明的目的,本发明提供一种水热炭负载纳米级零价镍催化剂的制备方法。通过在水热炭上负载纳米级的零价镍颗粒,制备了能够应用于市政污泥催化裂解气化的催化剂,该催化剂制备成本低,反应条件温和,催化活性高,具有良好的稳定性和催化寿命,能够显著提高合成气中氢气体积分数。该工艺的制备效果受前驱体浓度、水热炭化反应温度、反应时间、煅烧温度、气化温度、催化剂用量等因素的影响。
本发明的主要优点体现在以下几方面:
六水合硝酸镍溶液的浓度是1.0-1.5mol/L,其原因是:镍离子浓度过高,会导致镍离子在水热炭载体表面的过饱和吸附,在催化反应中导致大量表面活性位点的流失,降低催化反应活性。镍离子浓度过低,会导致镍离子在水热炭载体表面的不饱和吸附,减少催化剂表面活性位点数量,降低催化效率。
水热炭化温度选200-240℃,反应时间2-4h,其原因是:利用水热炭表面丰富的电子转移基团实现Ni2+向Ni0电子转移的Ni“自还原”过程。水热炭化温度过高或反应时间过长,水热炭表面电子转移基团种类和数量会显著降低,影响Ni“自还原”反应进程。水热炭化温度过低或反应时间过短,Ni纳米颗粒与水热炭载体的相互作用较弱,影响后续催化稳定性。
催化剂在700℃温度下煅烧2h,其原因是:煅烧温度过高或煅烧时间过长,会造成零价纳米镍颗粒尺寸的过度增长,减少活性晶面暴露数量,降低催化活性。煅烧温度过低或煅烧时间过短,零价纳米镍颗粒与水热炭载体之间的相互作用较弱,催化反应中容易流失活性组分,降低催化效率和催化稳定性。
在两段式催化反应系统中,将市政污泥样品在700-800℃进行水蒸气催化气化反应,其原因是:气化反应温度过高,容易导致催化剂活性中心烧结、失活,降低催化效率。气化反应温度过低,气化合成气中焦油副产物含量过高,降低焦油的催化裂解效率。
在市政污泥两段式气化反应过程中催化剂的用量为8-15wt.%,其原因是:催化剂用量过高,副产物产率增加,目标产物的产率及选择性降低。催化剂用量过低,催化反应活性不足,气化反应转化率较低,降低了目标产物的收率。
下面结合说明书附图及实施方案进一步阐述本发明的内容。
附图说明
图1生物质基功能纳米材料的制备及其用于市政污泥富氢气化的生产工艺流程示意图。
具体实施方式
本发明利用典型农业废弃物稻壳制备水热炭负载纳米级零价Ni催化剂,用于市政污泥的高效富氢气化。
实施案例一
1.生物质基功能纳米材料的制备
1)以典型农业废弃物稻壳为生物质废弃物原料,将其与1.2mol/L浓度的六水合硝酸镍溶液按1:4进行充分混合。
2)将稻壳与六水合硝酸镍溶液的混合物置入高压反应釜中,随后将反应器升温至220℃,反应时间为3h。
3)当到达反应停留时间后,通过自动循环水迅速冷却反应器,释放气相副产物,当反应器压力降低至常压后,将固液混合物通过离心进行固液分离,然后将固相产物在750℃温度下煅烧2h后最终获得水热炭负载零价纳米镍催化剂。
2.市政污泥的水蒸气催化气化反应
1)在两段式催化反应系统中,将市政污泥样品置入第一段热解区,将制备的水热炭基催化剂置入第二段催化重整区,密封整个气化系统后以N2吹扫整个系统以维持惰性气氛。
2)通过水蒸气发生器制备高温水蒸气作为气化反应介质,其中水蒸气温度为180℃。
3)将两段式催化反应系统升温至750℃后,将高温水蒸气通入气化反应器内,进行高温水蒸气气化反应,催化剂的用量为10wt.%。
4)将市政污泥水蒸气气化反应所得粗燃气进行净化除焦油后干燥,即可得到气化合成气,制备的气化合成气按照国标GB/T 10410-2008(人工煤气和液化石油气常量组分气相色谱分析法)标准或方法进行检测,检测结果如表1。
实施案例二
除了使用生物质废弃物稻壳作为催化剂前驱体,使用市政污泥作为催化气化反应原料;
生物质基功能纳米材料的制备中除了步骤1)将原始生物质废弃物稻壳与1.0mol/L浓度的六水合硝酸镍溶液按1:4进行混合;步骤2)水热炭化反应温度设为230℃,反应时间设为2h;步骤3)煅烧温度设为750℃之外,其余与实施案例一相同。
市政污泥水蒸气气化反应中除了步骤3)水蒸气气化温度为700℃,催化剂用量为8wt.%之外,其余与实施案例一相同。
气化粗燃气净化处理与实施案例一相同,制备的气化合成气按照国标GB/T10410-2008(人工煤气和液化石油气常量组分气相色谱分析法)标准或方法进行检测,检测结果如表1。
实施案例三
除了使用生物质废弃物稻壳作为催化剂前驱体,使用市政污泥作为催化气化反应原料;
生物质基功能纳米材料的制备中除了步骤1)将原始生物质废弃物稻壳与1.5mol/L浓度的六水合硝酸镍溶液按1:4进行混合;步骤2)水热炭化反应温度设为240℃,反应时间设为4h;步骤3)煅烧温度设为800℃之外,其余与实施案例一相同。
市政污泥水蒸气气化反应中除了步骤3)水蒸气气化温度为800℃,催化剂用量为15wt.%之外,其余与实施案例一相同。
气化粗燃气净化处理与实施案例一相同,制备的气化合成气按照国标GB/T10410-2008(人工煤气和液化石油气常量组分气相色谱分析法)标准或方法进行检测,检测结果如表1。
表1市政污泥气化合成气组分及焦油催化裂解率指标
项目 | 实施案例一 | 实施案例二 | 实施案例三 |
H2(%) | 81% | 73% | 71% |
CO(%) | 7% | 9% | 13% |
CH4(%) | 6% | 8% | 3% |
焦油催化裂解率(%) | 97.3% | 92.5% | 89.7% |
本发明的有益效果体现在以下方面:
1.本发明方法中以生物质废弃物稻壳为水热炭基催化剂前驱体,相对于传统负载型催化剂载体(如天然矿石、分子筛类),原料可再生且成本低廉,制备的生物质基功能纳米材料用于市政污泥的催化气化,实现市政污泥的清洁能源化转化,达到“以废治废”的效果。
2.本发明制备的气化合成气中氢气最高体积分数>80%,焦油催化裂解效率>95%。
3.本发明方法的新型制氢工艺路线,既能解决传统制氢工艺能耗大、成本高、环境污染严重的问题,又能解决市政污泥、农业废弃物稻壳等生物质废弃物带来的面源污染,具有一定的经济和社会效益。
Claims (7)
1.一种新型生物质基功能纳米材料的制备方法及其应用,其特征在于:以生物质废弃物稻壳为催化剂前驱体,与一定浓度的六水合硝酸镍混合,将混合物置入高压反应釜中进行水热炭化预处理,反应后离心分离固相产物,进行高温煅烧即可得到水热炭负载零价纳米镍催化剂,在两段式气化反应系统中通过市政污泥的催化气化反应可制备富氢气化合成气。
2.根据权利要求1所述的一种新型生物质基功能纳米材料的制备方法及其应用,其特征是:原始生物质废弃物稻壳与1.0-1.5mol/L浓度的六水合硝酸镍溶液按1:4进行水热炭化反应。
3.根据权利要求1所述的一种新型生物质基功能纳米材料的制备方法及其应用,其特征是:水热炭化温度200-240℃,反应时间2-4h。
4.根据权利要求1所述的一种新型生物质基功能纳米材料的制备方法及其应用,其特征是:催化剂在700-800℃下煅烧2h。
5.根据权利要求1所述的一种新型生物质基功能纳米材料的制备方法及其应用,其特征是:在两段式催化反应系统中,以水蒸气为气化介质,以制备的生物质基功能纳米材料为催化剂,将市政污泥样品在700-800℃中进行催化气化反应。
6.根据权利要求1所述的一种新型生物质基功能纳米材料的制备方法及其应用,其特征是:催化剂的用量为8-15wt.%。
7.根据权利要求1-6任意一项所述方法制备得到的富氢合成气,气化合成气中氢气体积分数>80%,焦油催化裂解效率>95%。
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