H_2气氛下碱活化石油焦制备活性炭及连续活化技术开发
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摘要
KOH活化法所制高比表面积活性炭微孔结构发达、吸附容量大,在燃料气存储、气体分离、催化反应及双电层电容器等方面具有巨大的应用前景。石油焦为炼油厂的副产物,其资源比较丰富,且其碳含量高(80wt%以上),灰分及挥发份含量低,是制备性能优良的活性炭的优良原料。但由于石油焦结晶度高,结构较为致密,活化比较困难,通常在惰性气氛下采用高碱焦比(KOH/石油焦质量比大于3：1)进行活化成孔。过高的碱焦比带来一系列问题,包括高碱耗、高污染、高成本,以及设备腐蚀、安全隐患等,从而制约了其开发与应用。在国内,KOH活化法制备石油焦基高比表面积活性炭技术多处于间歇式小试阶段,生产效率低,无法实现规模化生产。因此,开发一种连续化生产,碱用量较低,产品性能优良的石油焦生产活性炭的工艺技术及装备成为迫切需要解决的问题。基于此,本文着重开展了以下几方面的研究：
1.以实验室管式活化反应器为平台,以辽化石油焦为原料,以KOH为活化剂,通过在载气N2中引入活性气体H2制备出高比表面积活性炭。在活化过程中引入H2条件下,对碱焦比、活化温度、活化时间、载气中H2含量及石油焦粒度对活性炭孔隙结构及收率的影响进行了系统的考察。研究发现：(1)无论是在N2气氛下还是在N2+H2气氛下,碱焦比、活化温度、活化时间、载气中H2含量及石油焦粒度都会影响活性炭产品性能。(2)当碱焦比为2：1、活化温度为780℃、活化时间为60min、原料粒度为小于150μm以及载气中的H2含量为30%时,制备出的活性炭比表面积和孔容分别高达2477m2/g和1.10cm3/g。与在相同的条件下,未引入H2时制得的活性炭相比,比表面积和孔容分别提高了约500m2/g和0.25cm3/g。
2.通过在N2及N2+H2气氛对石油焦进行热处理,研究了载气中的H2在石油焦炭化过程中的作用。在载气引入H2有利于脱除石油焦表面的杂原子基团,从而使其炭化产物有着更低的氮、硫、氧元素含量,同时,H2又会与因脱除表面基团而形成的活性位发生化学吸附作用,形成-CH2-及芳环=CH-基团。
3.在N2及N2+H2气氛下进行KOH活化石油焦,通过分析其尾气中的H2含量、水蒸气的产生量、所制活性炭的元素组成及活化过程中钾单质的产量,研究了载气中H2在活化过程中的作用机理。活化过程中H2的引入会与石油焦表面官能团发生反应,造成尾气中H2的产生量减少,同时由于其与表面含氧官能团的作用,使活化过程的水的产生量增加。H2与石油焦表面杂原子基团作用所形成的-CH2-及芳环=CH-基团可作为活性位参与活化反应。活性位数量的增加,促进了活化反应的进行,同时产生的钾单质的量也进步增加,进一步促进了钾单质的插层活化作用。
4.采用经过HCl+HF进行脱灰处理过的石油焦为原料,在N2及N2+H2气氛下进行活化时发现,石油焦原料的灰分对H2活化几乎不起任何作用。采用不同表面性质的原料在N2及N2+H2气氛下进行活化时发现,当采用石墨为原料时,引入H2进行活化对孔隙结构的发展几乎不起任何作用,而采用其它含有一定量杂原子的原料进行活化时,引入H2对活性炭孔隙结构的发展均起着明显的促进作用。通过在活化过程中引入水蒸气活化实验发现,在引入H2进行活化时各个温度段多产生的水的量对最终活性炭的孔结构的发展并未产生明显的影响。
5.将N2及N2+H2气氛下所制活性炭应用于双电层电极材料,研究其电化学性能。当碱焦比为3：1、活化温度为780℃、活化时间为60min、原料粒度为小于150μm时,在载气引入30%的H2能够制备出比表面积及孔容分别高达2824m2/g和1.56cm3/g的活性炭。与在相同的条件下,未引入H2时制得的活性炭相比,比表面积、总孔容及中孔孔容分别提高了约400m2/g、0.40cm3/g和0.25cm3/g。将所制活性炭应用于双电层电容器电极材料,在所考察的扫描速率下,N2+H2气氛下所制活性炭电极材料的质量比电容均明显大于N2气氛下所制活性炭电极材料。
6.针对KOH活化的特点,构建由原料/KOH混合脱水、连续活化反应单元和钾脱插及转化单元三个主要部分串联的连续活化反应体系,并完成了连续活化反应装置的设计、建造及调试。采用该炉进行连续活化试验,所制活性炭性能已接近于固定床管式活化炉所制活性炭产品性能。通过对不同批次的活性炭孔结构分析可以看出,采用该炉制备的活性炭性能具有较好的稳定性。
Activated carbons (AC) produced by KOH activation are widely used in fuel gas separation, gas storage, catalysis reaction, electric double-layer capacitor (EDLC) materials and various chemical processes due to their developed micropore structure and larger pore volume. It is well known that petroleum coke (PC) is a good precursor for preparing high surface area AC because of its abundant resource, high carbon content, low volatile and ash content. However, PC is difficult to be activated due to the stable micro-graphitic structure. Generally, high KOH/PC ratio is needed to prepare AC from PC, which brings many problems, such as high KOH consumption, high pollution, high cost, equipment corrosion, hidden danger, and so on. These problems restrict the exploration and application of PC-based high surface area activated carbons. In domestic, the research on the production of AC from PC by the KOH activation is just in the batch production with the small scale device. This will cause the low production efficiency and restrict its large scale production. Therefore, how to explore a process technology with low KOH consumption and continuous equipment for the production of AC with high performance is the emphasis for further research. In this dissertation, investigations were conducted as follows:
AC was prepared from a green petroleum coke (PC) from SINOPEC Liaoyang Petrochemical Company and KOH as activating agent in the presence of Ho. The horizontal tube furnace was used for the activation. The effects of preparation variables including KOH/PC ratio, activation temperature, activation time, content of H2in the carrier gas and particle size of the PC on the porosity development of the AC were investigated. All the variables had an important influence on the performance of the AC. At the KOH/coke ratio of2:1, activation temperature780℃and activation time60min, AC with the specific surface area of2477m2/g and pore volume of1.10cm3/g was prepared in the presence of30%H2. The surface area and pore volume of the AC increased by500m2/g and0.25cm3/g, respectively, compared with that of AC prepared in the N2atmosphere.
The effects of H2on the carbonization of PC were investigated. The presence of H2is beneficial for removal of the surface heteroatom groups of the PC during the carbonization process, which caused the carbonized samples had a lower content of nitrogen, sulfur and oxygen. Meanwhile, additional-CH-and-CH2-species were formed due to the chemisorption of H2on the nascent sites of the PC created by the removal of the surface heteroatom groups.
The effects of H2on KOH activation of petroleum coke were systematically investigated by analyzing the evolution rate of H2, evolution of water, production of metallic K and element content of AC. The reaction of H2with the surface groups of PC caused the reduction of H2content in the sweep and the increase in the production of water. The formed-CH-and-CH2-species could act as 'active sites' to participate in the activation reaction. The increase in the quantity of'active sites'is beneficial to the further activation reaction. And the formation of metallic K could enhance the activation reaction.
The PC (deashed with hydrochloride acid and hydrofluoric acid), graphite and other carbon materials (with some surface groups) were adopted as the raw materials for the activation under N2and N2+H2atmosphere. The result showed that the ash in the PC almost has no effect on the KOH activation of PC. The introduction of H2in the carrier gas almost has no effect on the porosity development of AC prepared from graphite. But as the other carbon materials were used as raw material, the introduction of H2is beneficial for the porosity development of the AC. The water produced by the interaction of H2and suface oxygen groups of PC had no evident effect on the porosity development of the resultant activated carbon.
AC prepared from PC was used as electric double-layer capacitor (EDLC) materials. At the KOH/coke ratio of3:1, activation temperature780℃and activation time60min AC with specific surface area of2824m7g and pore volume of1.56cm/g was prepared in the presence of30%H2. The specific surface area, total pore volume and mesopore volume of the AC increased by400m2/g,0.40cm3/g and0.25cm3/g, respectively, compared with that of AC prepared in the N2atmosphere. At the investigated range of scanning rate, the gravimetric specific capacitance of the electric double-layer capacitor made from the AC prepared under H2+N2is higher than that prepared in the N2atmosphere.
Based on the characteristic of KOH activation, the continuous activation system was constructed which included the dehydration system, continuous activation system and metallic potassium convertion system. And the continuous activation device was designed, constructed and adjusted. The performance of AC prepared with the activation device is close to that prepared with horizontal pipe reactor. Porosity characterization of AC from different batches showed that the AC prepared with the activation device has a good stability.
1.以实验室管式活化反应器为平台,以辽化石油焦为原料,以KOH为活化剂,通过在载气N2中引入活性气体H2制备出高比表面积活性炭。在活化过程中引入H2条件下,对碱焦比、活化温度、活化时间、载气中H2含量及石油焦粒度对活性炭孔隙结构及收率的影响进行了系统的考察。研究发现：(1)无论是在N2气氛下还是在N2+H2气氛下,碱焦比、活化温度、活化时间、载气中H2含量及石油焦粒度都会影响活性炭产品性能。(2)当碱焦比为2：1、活化温度为780℃、活化时间为60min、原料粒度为小于150μm以及载气中的H2含量为30%时,制备出的活性炭比表面积和孔容分别高达2477m2/g和1.10cm3/g。与在相同的条件下,未引入H2时制得的活性炭相比,比表面积和孔容分别提高了约500m2/g和0.25cm3/g。
2.通过在N2及N2+H2气氛对石油焦进行热处理,研究了载气中的H2在石油焦炭化过程中的作用。在载气引入H2有利于脱除石油焦表面的杂原子基团,从而使其炭化产物有着更低的氮、硫、氧元素含量,同时,H2又会与因脱除表面基团而形成的活性位发生化学吸附作用,形成-CH2-及芳环=CH-基团。
3.在N2及N2+H2气氛下进行KOH活化石油焦,通过分析其尾气中的H2含量、水蒸气的产生量、所制活性炭的元素组成及活化过程中钾单质的产量,研究了载气中H2在活化过程中的作用机理。活化过程中H2的引入会与石油焦表面官能团发生反应,造成尾气中H2的产生量减少,同时由于其与表面含氧官能团的作用,使活化过程的水的产生量增加。H2与石油焦表面杂原子基团作用所形成的-CH2-及芳环=CH-基团可作为活性位参与活化反应。活性位数量的增加,促进了活化反应的进行,同时产生的钾单质的量也进步增加,进一步促进了钾单质的插层活化作用。
4.采用经过HCl+HF进行脱灰处理过的石油焦为原料,在N2及N2+H2气氛下进行活化时发现,石油焦原料的灰分对H2活化几乎不起任何作用。采用不同表面性质的原料在N2及N2+H2气氛下进行活化时发现,当采用石墨为原料时,引入H2进行活化对孔隙结构的发展几乎不起任何作用,而采用其它含有一定量杂原子的原料进行活化时,引入H2对活性炭孔隙结构的发展均起着明显的促进作用。通过在活化过程中引入水蒸气活化实验发现,在引入H2进行活化时各个温度段多产生的水的量对最终活性炭的孔结构的发展并未产生明显的影响。
5.将N2及N2+H2气氛下所制活性炭应用于双电层电极材料,研究其电化学性能。当碱焦比为3：1、活化温度为780℃、活化时间为60min、原料粒度为小于150μm时,在载气引入30%的H2能够制备出比表面积及孔容分别高达2824m2/g和1.56cm3/g的活性炭。与在相同的条件下,未引入H2时制得的活性炭相比,比表面积、总孔容及中孔孔容分别提高了约400m2/g、0.40cm3/g和0.25cm3/g。将所制活性炭应用于双电层电容器电极材料,在所考察的扫描速率下,N2+H2气氛下所制活性炭电极材料的质量比电容均明显大于N2气氛下所制活性炭电极材料。
6.针对KOH活化的特点,构建由原料/KOH混合脱水、连续活化反应单元和钾脱插及转化单元三个主要部分串联的连续活化反应体系,并完成了连续活化反应装置的设计、建造及调试。采用该炉进行连续活化试验,所制活性炭性能已接近于固定床管式活化炉所制活性炭产品性能。通过对不同批次的活性炭孔结构分析可以看出,采用该炉制备的活性炭性能具有较好的稳定性。
Activated carbons (AC) produced by KOH activation are widely used in fuel gas separation, gas storage, catalysis reaction, electric double-layer capacitor (EDLC) materials and various chemical processes due to their developed micropore structure and larger pore volume. It is well known that petroleum coke (PC) is a good precursor for preparing high surface area AC because of its abundant resource, high carbon content, low volatile and ash content. However, PC is difficult to be activated due to the stable micro-graphitic structure. Generally, high KOH/PC ratio is needed to prepare AC from PC, which brings many problems, such as high KOH consumption, high pollution, high cost, equipment corrosion, hidden danger, and so on. These problems restrict the exploration and application of PC-based high surface area activated carbons. In domestic, the research on the production of AC from PC by the KOH activation is just in the batch production with the small scale device. This will cause the low production efficiency and restrict its large scale production. Therefore, how to explore a process technology with low KOH consumption and continuous equipment for the production of AC with high performance is the emphasis for further research. In this dissertation, investigations were conducted as follows:
AC was prepared from a green petroleum coke (PC) from SINOPEC Liaoyang Petrochemical Company and KOH as activating agent in the presence of Ho. The horizontal tube furnace was used for the activation. The effects of preparation variables including KOH/PC ratio, activation temperature, activation time, content of H2in the carrier gas and particle size of the PC on the porosity development of the AC were investigated. All the variables had an important influence on the performance of the AC. At the KOH/coke ratio of2:1, activation temperature780℃and activation time60min, AC with the specific surface area of2477m2/g and pore volume of1.10cm3/g was prepared in the presence of30%H2. The surface area and pore volume of the AC increased by500m2/g and0.25cm3/g, respectively, compared with that of AC prepared in the N2atmosphere.
The effects of H2on the carbonization of PC were investigated. The presence of H2is beneficial for removal of the surface heteroatom groups of the PC during the carbonization process, which caused the carbonized samples had a lower content of nitrogen, sulfur and oxygen. Meanwhile, additional-CH-and-CH2-species were formed due to the chemisorption of H2on the nascent sites of the PC created by the removal of the surface heteroatom groups.
The effects of H2on KOH activation of petroleum coke were systematically investigated by analyzing the evolution rate of H2, evolution of water, production of metallic K and element content of AC. The reaction of H2with the surface groups of PC caused the reduction of H2content in the sweep and the increase in the production of water. The formed-CH-and-CH2-species could act as 'active sites' to participate in the activation reaction. The increase in the quantity of'active sites'is beneficial to the further activation reaction. And the formation of metallic K could enhance the activation reaction.
The PC (deashed with hydrochloride acid and hydrofluoric acid), graphite and other carbon materials (with some surface groups) were adopted as the raw materials for the activation under N2and N2+H2atmosphere. The result showed that the ash in the PC almost has no effect on the KOH activation of PC. The introduction of H2in the carrier gas almost has no effect on the porosity development of AC prepared from graphite. But as the other carbon materials were used as raw material, the introduction of H2is beneficial for the porosity development of the AC. The water produced by the interaction of H2and suface oxygen groups of PC had no evident effect on the porosity development of the resultant activated carbon.
AC prepared from PC was used as electric double-layer capacitor (EDLC) materials. At the KOH/coke ratio of3:1, activation temperature780℃and activation time60min AC with specific surface area of2824m7g and pore volume of1.56cm/g was prepared in the presence of30%H2. The specific surface area, total pore volume and mesopore volume of the AC increased by400m2/g,0.40cm3/g and0.25cm3/g, respectively, compared with that of AC prepared in the N2atmosphere. At the investigated range of scanning rate, the gravimetric specific capacitance of the electric double-layer capacitor made from the AC prepared under H2+N2is higher than that prepared in the N2atmosphere.
Based on the characteristic of KOH activation, the continuous activation system was constructed which included the dehydration system, continuous activation system and metallic potassium convertion system. And the continuous activation device was designed, constructed and adjusted. The performance of AC prepared with the activation device is close to that prepared with horizontal pipe reactor. Porosity characterization of AC from different batches showed that the AC prepared with the activation device has a good stability.
引文
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