甲烷低温等离子体活化与煤热解耦合过程研究
摘要
本文以实现CH4/C02低温活化并与煤热解制油最佳温度区间相匹配,从而提高CH4/CO2活化与煤热解耦合过程焦油产率为出发点,开展以下几方面的工作：
(1)探索和比较了多种用于CH4/CO2低温等离子体转化的介质阻挡放电(DBD)反应器形式,并选择了介质层位于低压电极侧的单层介质DBD反应器；对反应器的结构参数和工艺条件进行了优化。用设计的反应器进行C02转化实验表明：增大气体流量、提高原料气中CO2的含量或向反应气氛中添加Ar/H2有利于高温条件下放电的稳定进行；增加输入功率能显著提高气体的转化率；升高温度对C02转化有促进作用,但效果不明显,且会对放电稳定性产生较大影响。CH4等离子体中主要发生裂解出一个H·形成"CH3的反应。
(2)研究了各工艺条件对神木烟煤(SM)和霍林河褐煤(HLH)在CH4/CO2低温等离子体(P)活化与煤热解耦合过程中产物分布的影响。结果表明,向CH4/CO2中添加50%的H2形成混合气(MG),不仅能促进放电的稳定,还能获得较高的焦油产率；不同气氛对提高焦油产率的作用大致有如下顺序：MG-P> CH4-P≈CH4/H2-P≈CO2/H2-P>H2-P>H2>N2,在低温范围内(400～500。C)这种趋势更为明显；增大气体流量能促进放电的稳定和煤的转化,但水产率也随之增加,SM煤焦油产率随流量的增大而增加,而HLH煤则相反；在不影响放电稳定性的前提下,增加反应时间和输入功率有利于焦油产率的提高。
(3)采用H2等离子体直接处理法制备了Ni/SiO2催化剂,与传统先煅烧再加氢还原的工艺制备的催化剂相比,其具有更好的CH4/CO2催化重整活性和稳定性。研究了工艺条件对H2等离子体直接处理法制备的Ni/SiO2和Ni/Al2O3的催化重整与等离子体-催化重整性能的影响,发现等离子体-催化重整能促进Ni/Al2O3催化剂上CH4和CO2的转化；但对于Ni/SiO2,只能促进CO2的转化；等离子体放电条件下的液体产率高于不放电时的液体产率。将CH4/CO2催化重整和等离子体-催化重整过程分别与煤热解过程耦合(ICCC和ICCP),发现对ICCC过程来说,Ni/Al2O3催化剂和较高的热解温度或较长的反应时间有利于焦油产率的提高；对ICCP过程来说,Ni/SiO2催化剂、较低的温度范围、较短的反应时间、混合气中较高的H2含量以及较高的输入功率等条件有利于焦油产率的提高；催化剂Ni担载量对产物产率的影响较小。ICCC和ICCP过程的最高焦油产率分别为25.5%和23.7%,均高于相应条件的MG-P气氛下的焦油产率。
(4)对不同气氛下半焦的FT-IR分析表明：等离子体与煤之间确实存在着相互作用,不同气氛的等离子体与煤之间的相互作用不同。对焦油的1HNMR分析表明,H2-P气氛下,芳香氢含量升高,脂肪氢含量降低,而其它等离子体气氛下芳香氢含量降低,脂肪氢含量升高；13C NMR分析表明,CH4/H2-P、CO2/H2-P和MG-P气氛下,与3个H相连的饱和脂肪碳(CH3)含量升高,CO2/H2-P和MG-P气氛下,与-OH相连的芳香碳含量增加；等离子体气氛下,焦油的芳香度降低。对焦油的280℃前馏分的GC-MS和GC分析表明,其主要成分是酚、萘及它们的同系物；酚和萘的同系物中,C1和C2烷基取代物是主要的存在形式,且等离子体气氛下它们的相对含量更高。上述结果表明,等离子体气氛中丰富的H·、·CHx、·OH等自由基参与了焦油的形成,促进了焦油的轻质化。
(5)对耦合过程的能效分析表明,耦合过程平均每增产1g焦油需消耗有效放电能量约5.1Wh,仍存在改进空间。对等离子体放电的原位发射光谱诊断表明,等离子体中存在H、CH、C+等离子；模拟计算了放电条件下的气体转动温度和振动温度。耦合过程的同位素示踪显示,焦油的主要成分如苯酚、甲酚和萘中均能检测到不止1个D原子存在,说明耦合过程确实有CD4分解产生的自由基与煤热解自由基结合。
The main purpose of this dissertation was to explore a new process which can effectively activate methane under relatively low temperature and match the optimal temperature range during coal pyrolysis for high tar yield. The main research works and results are summarized as follows:
(1) Several kinds of dielectric barrier discharge (DBD) reactors were investigated for methane activation, and the optimum reactor with one dielectric layer located on the low-voltage electrode side was determined. The structural parameters of the reactor and reaction conditions were optimized to ensure that the discharge can be operated under high temperature. The results for CH4/CO2conversion in the designed DBD reactor show that increasing the gas flow rate, CO2content in the feed gas or adding Ar/H2to the feed gas can promote the stability of the discharge under high temperature; increasing the input power can remarkably increase the CH4and CO2conversion. However, increasing the temperature only has weak effect on increasing the CH4and CO2conversion and leads to the instability of the discharge. CH4molecule in DBD plasma are mainly dissociated to H-and-CH3.
(2) The effects of reaction conditions on the product yields in the integrated process of Shenmu (SM) subbituminous coal and Huolinhe (HLH) lignite pyrolysis with CH4/CO2activation by DBD plasma were investigated. The results showed that when50%H2was added to CH4/CO2(1:1) to form a mixed gas (MG), the stability of the discharge could be promoted and a high tar yield could be achieved. The effect of different atmospheres on increasing the tar yield is in the following order:MG-P> CH4-P≈CH4/H2-P≈CO2/H2-P> H2-P> H2> N2, especially at low temperature range (400～500℃). Increasing the gas flow rate is favorable for the discharge stability and can improve the coal conversion, but the water yield increases, too, the tar yield of SM coal increases while that of HLH lignite decreases. Increasing the pyrolysis time and the input power can increase the tar yield on condition that the discharge is stable.
(3) Ni/SiO2catalyst was prepared by exposing the precursor directly in H2plasma, and it shows better catalytic activity and stability compared with Ni/SiO2prepared by normal method in CO2reforming methane (CRM). The catalytic and plasma-catalytic performances of Ni/SiO2and Ni/Al2O3prepared by H2plasma were investigated and the results indicated that CH4and CO2conversion were improved in plasma-catalytic process compared with catalytic process on Ni/Al2O3, while only CO2conversion was improved in plasma-catalytic process on Ni/SiO2. The effect of reaction conditions on product yield in the integrated process of coal pyrolysis with CRM by catalyst (ICCC) or plasma-catalyst (ICCP) was investigated. The results showed that Ni/Al2O3catalyst and high reaction temperature, or long reaction time are beneficial to increase the tar yield in the ICCC, while Ni/SiO2catalyst, low reaction temperature, short reaction time, high H2content in the feed gas and high input power are good for the ICCP. The Ni loading amount has weak effect on product yield of both processes. The highest tar yield is25.5%and23.7%for the ICCC and ICCP, respectively, which is higher than the tar yield under MG plasma.
(4) The FT-IR analyses of chars under different atmospheres indicate that the interaction between coal and plasma does exist and it is different under different atmospheres. The1H NMR analyses of tar show that the aromatic hydrogen content decreases while the aliphatic hydrogen content increases under plasma atmospheres except that under H2plasma which has the reversed change.13C NMR analyses show that the content of the saturated aliphatic C to three H bond increases under CH4/H2-P, CO2/H2-P and MG-P atmosphere, the content of the aromatic C which bond to-OH increases under CO2/H2-P and MG-P atmosphere, and the aromaticity decreases under plasma atmospheres. The main components identified by GC-MS and quantified by GC in the volatile fraction (280℃) of tar are phenol, naphthalene and their Ci-C3alkyl-substitute homologues, in which C1-C2substitutes are the main forms. All these analyses suggest that the abundant H·,·CHX,·OH radicals exist in plasma involved in tar formation during coal pyrolysis and have effect on upgrading the coal tar.
(5) Analysis showed that the consumption of the effective discharge energy is about5.1Wh for1g of tar increment, which still need to be improved. Radicals like H, CH and C+are detected in plasma by Optical Emission Spectrum, and the rotational temperature and vibration temperature were analogue calculated according to the spectra. Isotope analysis of the tar formed in the integrated process show that more than one deuterium atom exists in the main component of tar, such as phenol, cresol and naphthalene, which indicates that the radicals decomposed from CD4(CH4) by plasma combined with those generated from coal in the integrated process.
(1)探索和比较了多种用于CH4/CO2低温等离子体转化的介质阻挡放电(DBD)反应器形式,并选择了介质层位于低压电极侧的单层介质DBD反应器；对反应器的结构参数和工艺条件进行了优化。用设计的反应器进行C02转化实验表明：增大气体流量、提高原料气中CO2的含量或向反应气氛中添加Ar/H2有利于高温条件下放电的稳定进行；增加输入功率能显著提高气体的转化率；升高温度对C02转化有促进作用,但效果不明显,且会对放电稳定性产生较大影响。CH4等离子体中主要发生裂解出一个H·形成"CH3的反应。
(2)研究了各工艺条件对神木烟煤(SM)和霍林河褐煤(HLH)在CH4/CO2低温等离子体(P)活化与煤热解耦合过程中产物分布的影响。结果表明,向CH4/CO2中添加50%的H2形成混合气(MG),不仅能促进放电的稳定,还能获得较高的焦油产率；不同气氛对提高焦油产率的作用大致有如下顺序：MG-P> CH4-P≈CH4/H2-P≈CO2/H2-P>H2-P>H2>N2,在低温范围内(400～500。C)这种趋势更为明显；增大气体流量能促进放电的稳定和煤的转化,但水产率也随之增加,SM煤焦油产率随流量的增大而增加,而HLH煤则相反；在不影响放电稳定性的前提下,增加反应时间和输入功率有利于焦油产率的提高。
(3)采用H2等离子体直接处理法制备了Ni/SiO2催化剂,与传统先煅烧再加氢还原的工艺制备的催化剂相比,其具有更好的CH4/CO2催化重整活性和稳定性。研究了工艺条件对H2等离子体直接处理法制备的Ni/SiO2和Ni/Al2O3的催化重整与等离子体-催化重整性能的影响,发现等离子体-催化重整能促进Ni/Al2O3催化剂上CH4和CO2的转化；但对于Ni/SiO2,只能促进CO2的转化；等离子体放电条件下的液体产率高于不放电时的液体产率。将CH4/CO2催化重整和等离子体-催化重整过程分别与煤热解过程耦合(ICCC和ICCP),发现对ICCC过程来说,Ni/Al2O3催化剂和较高的热解温度或较长的反应时间有利于焦油产率的提高；对ICCP过程来说,Ni/SiO2催化剂、较低的温度范围、较短的反应时间、混合气中较高的H2含量以及较高的输入功率等条件有利于焦油产率的提高；催化剂Ni担载量对产物产率的影响较小。ICCC和ICCP过程的最高焦油产率分别为25.5%和23.7%,均高于相应条件的MG-P气氛下的焦油产率。
(4)对不同气氛下半焦的FT-IR分析表明：等离子体与煤之间确实存在着相互作用,不同气氛的等离子体与煤之间的相互作用不同。对焦油的1HNMR分析表明,H2-P气氛下,芳香氢含量升高,脂肪氢含量降低,而其它等离子体气氛下芳香氢含量降低,脂肪氢含量升高；13C NMR分析表明,CH4/H2-P、CO2/H2-P和MG-P气氛下,与3个H相连的饱和脂肪碳(CH3)含量升高,CO2/H2-P和MG-P气氛下,与-OH相连的芳香碳含量增加；等离子体气氛下,焦油的芳香度降低。对焦油的280℃前馏分的GC-MS和GC分析表明,其主要成分是酚、萘及它们的同系物；酚和萘的同系物中,C1和C2烷基取代物是主要的存在形式,且等离子体气氛下它们的相对含量更高。上述结果表明,等离子体气氛中丰富的H·、·CHx、·OH等自由基参与了焦油的形成,促进了焦油的轻质化。
(5)对耦合过程的能效分析表明,耦合过程平均每增产1g焦油需消耗有效放电能量约5.1Wh,仍存在改进空间。对等离子体放电的原位发射光谱诊断表明,等离子体中存在H、CH、C+等离子；模拟计算了放电条件下的气体转动温度和振动温度。耦合过程的同位素示踪显示,焦油的主要成分如苯酚、甲酚和萘中均能检测到不止1个D原子存在,说明耦合过程确实有CD4分解产生的自由基与煤热解自由基结合。
The main purpose of this dissertation was to explore a new process which can effectively activate methane under relatively low temperature and match the optimal temperature range during coal pyrolysis for high tar yield. The main research works and results are summarized as follows:
(1) Several kinds of dielectric barrier discharge (DBD) reactors were investigated for methane activation, and the optimum reactor with one dielectric layer located on the low-voltage electrode side was determined. The structural parameters of the reactor and reaction conditions were optimized to ensure that the discharge can be operated under high temperature. The results for CH4/CO2conversion in the designed DBD reactor show that increasing the gas flow rate, CO2content in the feed gas or adding Ar/H2to the feed gas can promote the stability of the discharge under high temperature; increasing the input power can remarkably increase the CH4and CO2conversion. However, increasing the temperature only has weak effect on increasing the CH4and CO2conversion and leads to the instability of the discharge. CH4molecule in DBD plasma are mainly dissociated to H-and-CH3.
(2) The effects of reaction conditions on the product yields in the integrated process of Shenmu (SM) subbituminous coal and Huolinhe (HLH) lignite pyrolysis with CH4/CO2activation by DBD plasma were investigated. The results showed that when50%H2was added to CH4/CO2(1:1) to form a mixed gas (MG), the stability of the discharge could be promoted and a high tar yield could be achieved. The effect of different atmospheres on increasing the tar yield is in the following order:MG-P> CH4-P≈CH4/H2-P≈CO2/H2-P> H2-P> H2> N2, especially at low temperature range (400～500℃). Increasing the gas flow rate is favorable for the discharge stability and can improve the coal conversion, but the water yield increases, too, the tar yield of SM coal increases while that of HLH lignite decreases. Increasing the pyrolysis time and the input power can increase the tar yield on condition that the discharge is stable.
(3) Ni/SiO2catalyst was prepared by exposing the precursor directly in H2plasma, and it shows better catalytic activity and stability compared with Ni/SiO2prepared by normal method in CO2reforming methane (CRM). The catalytic and plasma-catalytic performances of Ni/SiO2and Ni/Al2O3prepared by H2plasma were investigated and the results indicated that CH4and CO2conversion were improved in plasma-catalytic process compared with catalytic process on Ni/Al2O3, while only CO2conversion was improved in plasma-catalytic process on Ni/SiO2. The effect of reaction conditions on product yield in the integrated process of coal pyrolysis with CRM by catalyst (ICCC) or plasma-catalyst (ICCP) was investigated. The results showed that Ni/Al2O3catalyst and high reaction temperature, or long reaction time are beneficial to increase the tar yield in the ICCC, while Ni/SiO2catalyst, low reaction temperature, short reaction time, high H2content in the feed gas and high input power are good for the ICCP. The Ni loading amount has weak effect on product yield of both processes. The highest tar yield is25.5%and23.7%for the ICCC and ICCP, respectively, which is higher than the tar yield under MG plasma.
(4) The FT-IR analyses of chars under different atmospheres indicate that the interaction between coal and plasma does exist and it is different under different atmospheres. The1H NMR analyses of tar show that the aromatic hydrogen content decreases while the aliphatic hydrogen content increases under plasma atmospheres except that under H2plasma which has the reversed change.13C NMR analyses show that the content of the saturated aliphatic C to three H bond increases under CH4/H2-P, CO2/H2-P and MG-P atmosphere, the content of the aromatic C which bond to-OH increases under CO2/H2-P and MG-P atmosphere, and the aromaticity decreases under plasma atmospheres. The main components identified by GC-MS and quantified by GC in the volatile fraction (280℃) of tar are phenol, naphthalene and their Ci-C3alkyl-substitute homologues, in which C1-C2substitutes are the main forms. All these analyses suggest that the abundant H·,·CHX,·OH radicals exist in plasma involved in tar formation during coal pyrolysis and have effect on upgrading the coal tar.
(5) Analysis showed that the consumption of the effective discharge energy is about5.1Wh for1g of tar increment, which still need to be improved. Radicals like H, CH and C+are detected in plasma by Optical Emission Spectrum, and the rotational temperature and vibration temperature were analogue calculated according to the spectra. Isotope analysis of the tar formed in the integrated process show that more than one deuterium atom exists in the main component of tar, such as phenol, cresol and naphthalene, which indicates that the radicals decomposed from CD4(CH4) by plasma combined with those generated from coal in the integrated process.
引文
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