CN101868519A - 一种避免挥发性裂解产物在高温分解和气化期间发生聚合的工艺 - Google Patents

一种避免挥发性裂解产物在高温分解和气化期间发生聚合的工艺 Download PDF

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CN101868519A
CN101868519A CN200880109606A CN200880109606A CN101868519A CN 101868519 A CN101868519 A CN 101868519A CN 200880109606 A CN200880109606 A CN 200880109606A CN 200880109606 A CN200880109606 A CN 200880109606A CN 101868519 A CN101868519 A CN 101868519A
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马诺吉·库马尔·萨卡尔
巴尼布拉塔·潘迪
马莱彦迪·法三提
克鲁普若鲁·凡卡塔·劳
贝蒂奇姆叔·萨克斯普利亚
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Abstract

本发明旨在提供一种制备催化碳质材料、以及避免挥发性裂解产物在碳质材料的高温分解或气化期间发生聚合的工艺。

Description

一种避免挥发性裂解产物在高温分解和气化期间发生聚合的工艺
技术领域
本发明属于气化技术领域。
背景技术
生物质气化是一种由若干基本化学反应组成的复杂的热化学过程，该过程始于使用气化剂进行的木质纤维燃料的部分氧化，所用气化剂通常为空气、氧气或蒸汽。
生物质+O2(或H2O)→CO+CO2+H2O+H2+CH4+其他气态烃+焦油+灰分
在气化工艺中，碳质材料在不同的温度范围内(即从室温至1000℃)发生不同的化学反应。反应性质如下：
在400℃-600℃：碳质材料分解为烧焦物和挥发性物质。
在600℃-1000℃：碳与氧气反应，产生二氧化碳和热，且由此生成的CO2随后与C(烧焦物)反应，生成CO。
在1000℃：使用蒸汽调节温度，且所用蒸汽与碳反应，生成一氧化碳和氢气。
在400℃-600℃形成焦油，其中挥发性物质发生二次分解和聚合，生成焦油。由于若干原因，焦油在综合性生物质气化***中是一个难题。焦油会在出口管中和微粒过滤器上凝结，从而导致过滤器阻塞以及其他复杂化问题。如前上述，现有气化工艺利用很复杂和昂贵的净化***克服焦油问题。
例如以下一些技术已经过测试，并取得一定程度的成功：机械方法(洗涤器、过滤器、旋风分离器、ESP和RSP)、自修改方法(选择更好的气化器，并使操作参数最优化)、以及最近开发的等离子体技术。
机械方法只能从产物气体中除去或捕获焦油，但失去焦油中的能量。自修改方法可还原焦油，并将焦油转化为有用的气体；然而，修改操作参数是以减小气体热值为代价的。一种新的两级气化器可生成具有低焦油含量和高热值的合成气。
热裂解和催化裂解用于分解或减少焦油，可是仍存在一些缺点。为获得高效的焦油分解，需要很高的热裂解温度，由此会增加操作成本。催化剂裂解可在很低的温度下改变产物气体的成分。
对于催化剂裂解，例如存在以下缺点，即商品Ni基和碱金属催化剂将会由于沉积碳和H2S而具有惰性；对于白云石催化剂，微粒破碎也使活性降低。等离子体技术不仅能有效除去飞尘、NOx和SO2，也能在生物质气化期间大幅度减少焦油的形成。新颖的生物质内催化沉积(在生物质与催化剂之间发生最紧密接触)方法可克服这些缺点。
美国专利20070000177A1描述了碳质材料的低温催化气化工艺在燃料应用中可在温和温度下实现碳向甲烷的高转化。
美国专利7132183描述了碳质原料在一种气化器中的气化工艺，该工艺的高温操作范围为700℃-1600℃，且由于燃料电池中的电化学氧化而在该气化器中生成一部分气体。
专利WO20070044342描述了对由气化反应生成的气体中所含焦油的催化重整作用，该气化反应使用化学品吸收气体中所含的CO2，从而由于可流动的热载体和化学品的热传导而起到加速作用。
专利WO2006031011提供了一种气化技术，该气化技术包括第一阶段的流化床催化气化、以及第二阶段的焦油气化和催化重整，以将焦油中的氮和可燃气体中的HCN转化为NH3。整个工艺的温度低于灰分的熔点；且生成粉状灰，因而易于处理。
人们对于发展无焦油气化工艺、以将煤或生物质转化为合成气，已进行了广泛的研究。焦油生成工艺的难题在于导致焦油形成所涉及的反应机理。迄今为止，所有技术均涉及在气体生成之后除去在气化器外焦油的焦油去除操作。然而，尚没有技术用于避免在气化期间的高温分解步骤中焦油的形成。
发明目的
本发明的目的是避免挥发性裂解产物在高温分解和气化工艺期间发生聚合，由此避免在所述工艺期间形成焦油。
发明内容
因此，本发明旨在提供一种制备碳质材料的工艺，该碳质材料可用作高温分解和/或气化的起始物料，由此可消除焦油的形成。
一方面，本发明公开了一种制备催化碳质材料的工艺，所述工艺包括下列步骤：
(a)将碳质材料浸泡在可溶性金属盐溶液中；
(b)干燥步骤(a)中的碳质材料；以及
(c)将碳质材料的温度升高至足以使金属盐分解为其氧化物和/或碳酸盐的温度，以获得催化碳质材料。
其中，所述可溶性盐能够在低于碳质材料分解温度的温度下，分解为氧化物和/或碳酸盐。
另一方面，碳质材料是木质纤维生物质。
又一方面，金属盐选自含有镍、钴、铁和锌的群组。
在本工艺中使用的可溶性盐为碳酸镍酰铵(nickel ammonium carbonate)。
再一方面，本工艺中金属盐的浓度在0.05％-2％的范围内。
可溶性盐的分解温度在150℃-300℃的范围内。
在本发明的另一实施例中，本发明公开了一种避免挥发性裂解产物在碳质材料的高温分解或气化期间发生聚合的工艺，所述工艺包括热解和/或气化由本发明的第一实施例中公开的工艺制得的催化碳质材料。
在本发明中，填充床反应器用于气流上升式方式中，其中在底部流过反应性气体和氮气，在顶部释放产物气体。催化生物质的热解气化工艺是通过单独使用常规的重整试剂，即氧气、二氧化碳和蒸汽而进行的，或将这些气体与氮气组合使用。
具体实施方式
实施例
例1
原生物质在不同温度下的热解气化。
填充床空反应器被预热至高于反应温度40℃-50℃。一旦达到温度，在反应器中随后装入10g粗甜高粱蔗渣粒料。反应在450℃、500℃、550℃、600℃和650℃温度(反应温度)下进行。反应是在不同气体组合的情况下进行的，其中二氧化碳的流量为10L/hr，氧气的流量为二氧化碳的20％，蒸汽的流量为100ml/hr，氮气的流量保持在10L/hr。来自反应器的以蒸汽形式存在的液体分解产物被收集在用于估计焦油和液体产物的异丙醇介质中。在反应完成后，冷却反应器，并对烧焦物进行定量。结果示于表1。
表1给出焦油、烧焦物和液体产物在不同温度下的生成结果。
表1
Figure GPA00001077270700061
例2
0.1％镍催化剂对焦油去除的影响
填充床空反应器被预热至高于反应温度40℃-50℃。一旦达到温度，在反应器中随后装入10g催化甜高粱蔗渣粒料。反应在450℃、500℃、550℃、600℃和650℃温度(反应温度)下进行。反应是在不同气体组合的情况下进行的，其中二氧化碳的流量为10L/hr，氧气的流量为二氧化碳的20％，蒸汽的流量为100ml/hr，氮气的流量保持在10L/hr。来自反应器的以蒸汽形式存在的液体分解产物被收集在用于按下列步骤估计焦油和液体产物的异丙醇介质中。在反应完成后，冷却反应器，并对烧焦物进行定量。
收集在异丙醇中的液体是蒸汽，该蒸汽被蒸馏，以除去异丙醇和其他挥发性有机化合物。假定焦油为非挥发性，并留在残余水中。使用苯萃取焦油。
在蒸发苯和对作为焦油的残余物质秤重后，并对其进行定量。
结果示于表2。
表2给出焦油、烧焦物和液体产物在不同温度下的生成结果。
表2
例3
0.25％镍催化剂对焦油去除的影响
填充床空反应器被预热至高于反应温度40℃-50℃。一旦达到温度，在反应器中随后装入10g催化甜高粱蔗渣粒料。反应在450℃、500℃、550℃、600℃和650℃温度(反应温度)下进行。反应是在不同气体组合的情况下进行的，其中二氧化碳的流量为10L/hr，氧气的流量为二氧化碳的20％，蒸汽的流量为100ml/hr，氮气的流量保持在10L/hr。来自反应器的以蒸汽形式存在的液体分解产物被收集在用于估计焦油和液体产物的异丙醇介质中。在反应完成后，冷却反应器，并对烧焦物进行定量。结果示于表3。
表3给出焦油、烧焦物和液体产物在不同温度下的生成结果。
表3
Figure GPA00001077270700081
例4
0.5％镍催化剂对焦油去除的影响
填充床空反应器被预热至高于反应温度40℃-50℃。一旦达到温度，在反应器中随后装入10g催化甜高粱蔗渣粒料。反应在450℃、500℃、550℃、600℃和650℃温度(反应温度)下进行。反应是在不同气体组合的情况下进行的，其中二氧化碳的流量为10L/hr，氧气的流量为二氧化碳的20％，蒸汽的流量为100ml/hr，氮气的流量保持在10L/hr。来自反应器的以蒸汽形式存在的液体分解产物被收集在用于估计焦油和液体产物的异丙醇介质中。在反应完成后，冷却反应器，并对烧焦物进行定量。结果示于表4。
表4给出焦油、烧焦物和液体产物在不同温度下的生成结果。
表4
Figure GPA00001077270700091
例5
对在650℃热解气化得到的液体产物的分析
使用GC-MS对蒸汽蒸馏液体的有机液体层进行分析。
该分析显示该液体中含有诸如脂族醇、醛、酸、酚、酚和苯的衍生物、甲苯、糠醛和醛醣的成分。这表明该液体中不含焦油。
1.GC-MS的操作参数：
型号：5975，由Aglient制造
载气：氦气
流量：0.8ml/min
喷射器温度：220℃
柱：HP-5MS 5％苯基甲基硅氧烷(毛细管)
炉温：升温：5分钟达到40℃，8℃每分钟；
      最终温度为250℃，保持5分钟
电子枪：钨丝
离子源：电子轰击电离
质量分析器：四极质量分析器
MS四极温度：150℃
探测器：电子倍增管。
例6
对在650℃热解气化气体的成分分析
使用Nucon气体分析器分析来自反应器的气体。该分析器可对H2、CO2、CH4和CO的体积浓度进行测量。
表5给出在650℃热解气化气体的成分结果。
表5
  气体成分   ％
  CO   22.9
  CO2   21.4
  H2   15
  CH4   6.5

Claims (7)

1.一种制备催化碳质材料的工艺，所述工艺包括下列步骤：
(a)将碳质材料浸泡在可溶性金属盐溶液中；
(b)干燥步骤(a)中的所述碳质材料；以及
(c)将所述碳质材料的温度升高至足以使所述金属盐分解为其氧化物和/或碳酸盐的温度，以获得催化碳质材料；
其中：所述可溶性盐能够在低于所述碳质材料分解温度的温度下，分解为氧化物和/或碳酸盐。
2.根据权利要求1所述的工艺，其中：所述碳质材料是木质纤维生物质。
3.根据权利要求1所述的工艺，其中：所述金属盐选自包含镍、钴、铁和锌的群组。
4.根据权利要求1所述的工艺，其中：所述可溶性盐是碳酸镍酰铵(nickel ammonium carbonate)。
5.根据权利要求1所述的工艺，其中：金属盐的浓度在0.05％-2％的范围内。
6.根据权利要求1所述的工艺，其中：所述可溶性盐的分解温度在150℃-300℃的范围内
7.一种避免挥发性裂解产物在碳质材料的高温分解或气化期间发生聚合的工艺，所述工艺包括热解和/或气化根据权利要求1的所述工艺获得的催化碳质材料。
CN200880109606A 2007-08-01 2008-07-31 一种避免挥发性裂解产物在高温分解和气化期间发生聚合的工艺 Pending CN101868519A (zh)

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